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[ CAS No. 109-81-9 ] {[proInfo.proName]}

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Chemical Structure| 109-81-9
Chemical Structure| 109-81-9
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Product Details of [ 109-81-9 ]

CAS No. :109-81-9 MDL No. :MFCD00008165
Formula : C3H10N2 Boiling Point : -
Linear Structure Formula :H2NC2H4NHCH3 InChI Key :KFIGICHILYTCJF-UHFFFAOYSA-N
M.W : 74.12 Pubchem ID :8014
Synonyms :

Safety of [ 109-81-9 ]

Signal Word:Danger Class:8,3
Precautionary Statements:P280-P305+P351+P338-P310 UN#:2734
Hazard Statements:H225-H314 Packing Group:Ⅱ
GHS Pictogram:

Application In Synthesis of [ 109-81-9 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 109-81-9 ]

[ 109-81-9 ] Synthesis Path-Downstream   1~9

  • 1
  • [ 2002-24-6 ]
  • [ 593-51-1 ]
  • [ 109-01-3 ]
  • [ 109-81-9 ]
  • 2
  • [ 109-81-9 ]
  • [ 67104-97-6 ]
YieldReaction ConditionsOperation in experiment
52.3% With pyridine; imidosulfonic acid; for 3h;Reflux; N-methylethylendiamine (1.5 g, 20.8 mmol) and sulfuric diimide (2.0 g, 20.8 mmol) were added to a pyridinesolvent (20 mL), and refluxed, stirred, and heated for 3 hours. After the reaction was completed, toluene (5 mL) wasadded to the reactant, followed by concentration and extraction with ethyl acetate. An organic solvent layer was driedover MgSO4 and filtered to remove the solvent. A residue was purified by column chromatography (EtOAc) to obtain acompound 6a. White solid (52.3 %). Mp 80 to 82 C; 1H-NMR (CDCl3, 300 MHz) delta7.27 (s, 1H), 3.53-3.19 (m, 2H), 3.42-3.37 (m, 2H), 2.75 (s, 1H); 13C NMR (CDCl3, 75 MHz) delta 32.67, 39.64, 46.94; LC-MS: Predicted value calculated with respect to C3H8N2O2S m/z: 136. Measured value: 137(M+1)+.
28% With pyridine; SULFAMIDE; at 120℃; for 16h; Preparation 98 2-Methyl-1,2,5-thiadiazolidine-1,1-dioxide To a stirred mixture of N-methylethylenediamine (1.200 g, 16.2 mmol) in pyridine (20 mL) was added sulfamide (1.867 g, 19.4 mmol). The mixture was heated in an oil bath at 120 C. for 16 hrs. After cooling to room temperature, the mixture was concentrated and the residue was partitioned between ethyl acetate and saturated aqueous sodium chloride. The organic layer was washed with 1 N aqueous hydrochloric acid, saturated aqueous sodium chloride, dried (anhydrous sodium sulfate), filtered, and concentrated to afford a colorless oil (0.61 g, 28%). 1H NMR (300 MHz, CDCl3) delta 4.30 (br s, 1H), 3.53 (m, 2H), 3.40 (m, 2H), 2.76 (s, 3H).
16% With SULFAMIDE; In 1,4-dioxane; for 20h;Reflux; Step a) 2-Methyl-?.2.51thiadiazolidine 1.1 -dioxide (Acid-12a); N-Methylethylene diamine (1.02 ml, 11.6 mmol) in dioxane (4 ml) was added dropwise to sulphamide (1.12 g, 11.6 mmol) in dioxane (10 ml) over 2 h. The mixture was refluxed for 18 h, solvent evaporated and residue purified by flash chromatography using 3% MeOH in DCM as eluent which gave the title compound (259 mg, 16%) as a semisolid.
799.4 mg With pyridine; SULFAMIDE; at 120℃; for 24h;Inert atmosphere; To a solution of N1-methylethane-1,2-diamine (2.0 g, 27 mmol) in pyridine (30 mL) was added sulfuric diamide (3.10 g, 32.4 mmol). The reaction was heated at 120 C under nitrogen for 24 h. All solvents were removed in vacuo. The residue was partitioned between saturated NaCl (aq, 25 mL) and EtOAc (125 mL) and organic component was washed with IN HC1 (aq, 50 mL) and saturated NaCl (aq, 25 mL). The organic component was dried over MgS04, filtered, and concentrated in vacuo to afford the title compound as a yellow viscous oil (799.4 mg). The product was used without further purification. NMR (400 MHz, CDCh) delta 4.48 (br s, 1H), 3.59 - 3.45 (m, 2H), 3.44 - 3.33 (m, 2H), 2.75 (s, 3H).
2.7 g With pyridine; SULFAMIDE; at 100℃; for 16h; To a mixture of sulfamide (5 g, 52.1 mmol) in pyridine (120 mL) was added a solution of n-methylethylenediamine (3.85 g, 52.1 mmol) in pyridine (30 mL) at 100 C. The mixture was stirred at 100 C for 16 hours, and then concentrated under reduced pressure. The residue was purified by column chromatography to give intermediate 1-17 (2.7 g) as a colorless oil. 1H NMR (400 MHz, CDC13) delta 4.37 (brs, 1 H), 4.45-4.58 (m, 2 H), 3.34-3.42 (m, 2H), 2.76 (s, 3H).

  • 3
  • [ 16611-67-9 ]
  • [ 109-81-9 ]
  • [ 2898-12-6 ]
  • 4
  • [ 1458-01-1 ]
  • [ 109-81-9 ]
  • [ 119646-69-4 ]
YieldReaction ConditionsOperation in experiment
In tetrahydrofuran; (1) A mixture of 20 g (99.0 mmol) of methyl 3,5-diamino-6-chloropyrazine-2-carboxylate (see U.S. Pat. No. 4,029,816 for an example of how to obtain this material) and 17 g (230.0 mmol) of N-methylethylenediamine was heated at reflux under an inert atmosphere for 30 hours. The rection mixture was cooled to ambient temperature and the solid was dissolved in 100 ml of tetrahydrofuran. The solution was filtered and evaporated. The residue was crystallized from 2-propanol. There was obtained 15.0 g (61.2 mmol, 61percent) of 3,5-diamino-6-chloro-N-(2-methylaminoethyl)pyrazine-2-carboxamide; mp 142.5°-143° C. Analysis calculated for; C8 H13 ClN6 O: C, 39.27; H, 5.35; N, 34.35; Found: C, 39.28; H, 5.26; N, 34.55.
  • 5
  • [ 61929-24-6 ]
  • [ 109-81-9 ]
  • N1-methyl-N1-(1,3,4-thiadiazol-2-yl)ethane-1,2-diamine [ No CAS ]
YieldReaction ConditionsOperation in experiment
33% With copper; copper(l) chloride; In isopropyl alcohol; at 70℃; for 1h; a) Synthesis of N1-methyl-N1-(1,3,4-thiadiazol-2-yl)ethane-1,2-diamine 70 mg (1.1 mmol) copper and 328 mg (3.3 mmol) copper(I) chloride were added to a solution of 3.3 g (20.0 mmol) 2-bromothiadiazol and 10.6 ml (120.0 mmol) N-methyl-ethylene-diamine in isopropanol (114 ml). Heating was subsequently performed at 1 h to 70 C. After cooling to RT, filtration was performed through silica gel and the filtrate was concentrated in a vacuum. 1.05 g (6.6 mmol, 33%) N1-methyl-N1-(1,3,4-thiadiazol-2-yl)ethane-1,2-diamine was obtained by CC (DCE/EtOH/conc. aq. NH4OH sol. 4:4:0.25) with the residue.
  • 7
  • [ 21524-39-0 ]
  • [ 85290-78-4 ]
  • [ 109-81-9 ]
  • [ 1307314-30-2 ]
  • C17H19FN4O2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
A mixture of 3 -methyl- lH-pyrazole-4-carboxylic acid ethyl ester (1.25 g, 8.1 1 mmol), potassium carbonate (1.68 g, 12.16 mmol), 2,3-difluorobenzonitrile (1.08 mL, 9.73 mmol) in dimethylformamide (12 mL) is heated at 100C with the aid of a magnetic stirred. After 2.5 hr. the reaction mixture is treated with water and extracted with ethyl acetate. The organic layer is decanted, washed with brine, dried over magnesium sulfate and the solvent evaporated under reduced pressure to give 2.3 g of l-(2-cyano-6-fluoro- phenyl)-3 -methyl- lH-pyrazole-4-carboxylic acid ethyl ester (this compound is contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 274 (M+1). A capped vial is charged with ethyl l-(2-cyano-6-fluoro-phenyl)-3-methyl- pyrazole-4-carboxylate (1.97 g, 7.21 mmol) (contaminated with the other pyrazole regioisomer in a ratio of 75:25, 1,2-ethanediamine, N-methyl- (6 mL, 68.02 mmol) and phosphorus pentasulfide (229 mg, 1,01 mmol) and the mixture is stirred at 1 10C for 30 min and then allow to reach rt. Solvent is evaporated in vacuo and the residue purified by normal phase Isco chromatography using dichloromethane/2M ammonia in methanol from 95/5 to 85/15 as eluent to yield 2.1 1 g of ethyl l-[2-fluoro-6-(l-methyl-4,5- dihydroimidazol-2-yl)phenyl]-3-methyl-pyrazole-4-carboxylate (contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 331 (M+1).
  • 8
  • [ 21524-39-0 ]
  • [ 85290-78-4 ]
  • [ 109-81-9 ]
  • [ 1307314-31-3 ]
  • C17H17FN4O2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
A mixture of 3 -methyl- lH-pyrazole-4-carboxylic acid ethyl ester (1.25 g, 8.1 1 mmol), potassium carbonate (1.68 g, 12.16 mmol), 2,3-difluorobenzonitrile (1.08 mL, 9.73 mmol) in dimethylformamide (12 mL) is heated at 100C with the aid of a magnetic stirred. After 2.5 hr. the reaction mixture is treated with water and extracted with ethyl acetate. The organic layer is decanted, washed with brine, dried over magnesium sulfate and the solvent evaporated under reduced pressure to give 2.3 g of l-(2-cyano-6-fluoro- phenyl)-3 -methyl- lH-pyrazole-4-carboxylic acid ethyl ester (this compound is contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 274 (M+1). A capped vial is charged with ethyl l-(2-cyano-6-fluoro-phenyl)-3-methyl- pyrazole-4-carboxylate (1.97 g, 7.21 mmol) (contaminated with the other pyrazole regioisomer in a ratio of 75:25, 1,2-ethanediamine, N-methyl- (6 mL, 68.02 mmol) and phosphorus pentasulfide (229 mg, 1,01 mmol) and the mixture is stirred at 1 10C for 30 min and then allow to reach rt. Solvent is evaporated in vacuo and the residue purified by normal phase Isco chromatography using dichloromethane/2M ammonia in methanol from 95/5 to 85/15 as eluent to yield 2.1 1 g of ethyl l-[2-fluoro-6-(l-methyl-4,5- dihydroimidazol-2-yl)phenyl]-3-methyl-pyrazole-4-carboxylate (contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 331 (M+1). Potassium permanganate (1.58 g, 10 mmmol) and montmorillonite K- 10 (3.16 g) are grounded together in a mortar until a fine homogeneous powder is obtained.KMn04-montmorillonite K-10 (3.2 g, 6.78 mmol) is added portionwise to a solution of ethyl l-[2-fluoro-6-(l-methyl-4,5-dihydroimidazol-2-yl)phenyl]-3-methyl-pyrazole-4- carboxylate (1.12 g, 3.39 mmol) (contaminated with the other pyrazole regioisomer in a ratio 75:25) in acetonitrile (84.76 mL, 1.62 moles). The mixture is stirred at room temperature for 6.5 hr. and more KMn04-montmorillonite K-10 (0.8 g, 1.69 mmol) is added portionwise and the mixture stirred at room temperature overnight. Ethanol is added and stirred for additional 20 min. Then the reaction mixture is filtered through a short pad of celite and the solid material is washed with acetonitrile. The solvent is evaporated under reduced pressure and the crude mixture is purified normal phase Isco chromatography using ethyl acetate as eluent to yield 518 mg of l-[2-fluoro-6-(l- methylimidazol-2-yl)phenyl]-3-methyl-pyrazole-4-carboxylate (contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 329 (M+1).
  • 9
  • [ 21524-39-0 ]
  • [ 1307248-44-7 ]
  • [ 85290-78-4 ]
  • [ 109-81-9 ]
  • [ 1307313-52-5 ]
YieldReaction ConditionsOperation in experiment
A mixture of 3 -methyl- lH-pyrazole-4-carboxylic acid ethyl ester (1.25 g, 8.1 1 mmol), potassium carbonate (1.68 g, 12.16 mmol), 2,3-difluorobenzonitrile (1.08 mL, 9.73 mmol) in dimethylformamide (12 mL) is heated at 100C with the aid of a magnetic stirred. After 2.5 hr. the reaction mixture is treated with water and extracted with ethyl acetate. The organic layer is decanted, washed with brine, dried over magnesium sulfate and the solvent evaporated under reduced pressure to give 2.3 g of l-(2-cyano-6-fluoro- phenyl)-3 -methyl- lH-pyrazole-4-carboxylic acid ethyl ester (this compound is contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 274 (M+1). A capped vial is charged with ethyl l-(2-cyano-6-fluoro-phenyl)-3-methyl- pyrazole-4-carboxylate (1.97 g, 7.21 mmol) (contaminated with the other pyrazole regioisomer in a ratio of 75:25, 1,2-ethanediamine, N-methyl- (6 mL, 68.02 mmol) and phosphorus pentasulfide (229 mg, 1,01 mmol) and the mixture is stirred at 1 10C for 30 min and then allow to reach rt. Solvent is evaporated in vacuo and the residue purified by normal phase Isco chromatography using dichloromethane/2M ammonia in methanol from 95/5 to 85/15 as eluent to yield 2.1 1 g of ethyl l-[2-fluoro-6-(l-methyl-4,5- dihydroimidazol-2-yl)phenyl]-3-methyl-pyrazole-4-carboxylate (contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 331 (M+1). Potassium permanganate (1.58 g, 10 mmmol) and montmorillonite K- 10 (3.16 g) are grounded together in a mortar until a fine homogeneous powder is obtained.KMn04-montmorillonite K-10 (3.2 g, 6.78 mmol) is added portionwise to a solution of ethyl l-[2-fluoro-6-(l-methyl-4,5-dihydroimidazol-2-yl)phenyl]-3-methyl-pyrazole-4- carboxylate (1.12 g, 3.39 mmol) (contaminated with the other pyrazole regioisomer in a ratio 75:25) in acetonitrile (84.76 mL, 1.62 moles). The mixture is stirred at room temperature for 6.5 hr. and more KMn04-montmorillonite K-10 (0.8 g, 1.69 mmol) is added portionwise and the mixture stirred at room temperature overnight. Ethanol is added and stirred for additional 20 min. Then the reaction mixture is filtered through a short pad of celite and the solid material is washed with acetonitrile. The solvent is evaporated under reduced pressure and the crude mixture is purified normal phase Isco chromatography using ethyl acetate as eluent to yield 518 mg of l-[2-fluoro-6-(l- methylimidazol-2-yl)phenyl]-3-methyl-pyrazole-4-carboxylate (contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 329 (M+1). 4. Gamma 1 - r2-Fruoro-6-C 1 -methylimidazol-2-yl phenyl1-3 -methyl-pyrazol-4-yllmethanolThis compound is essentially prepared as described in Preparation 29 by using ethyl l-[2-fluoro-6-(l-methylimidazol-2-yl)phenyl]-3-methyl-pyrazole-4-carboxylate (contaminated with the other pyrazole regioisomer in a ratio 75:25) in 99% yield. MS (m/z): 287 (M+l).5. l-r2-Fluoro-6-(l-methylimidazol-2-yl phenyl1-3-methyl-pyrazole-4-carbaldehvdeThe following compound is essentially prepared as described in Preparation 30 by using [l-[2-fluoro-6-(l-methylimidazol-2-yl)phenyl]-3-methyl-pyrazol-4-yl]methanol (contaminated with the other pyrazole regioisomer in a ratio 75:25). Residue is purified by normal phase Isco chromatography using ethyl acetate as eluent to give 64% yield of the title compound (contaminated with the other pyrazole regioisomer in a ratio 75:25). MS (m/z): 285 (M+l). To a screw-cap test tube containing a mixture of l-[2-fluoro-6-(l- methylimidazol-2-yl)phenyl]-3-methyl-pyrazole-4-carbaldehyde (288 mg, 1.01 mmol) (contaminated with the other pyrazole regioisomer in a ratio 75:25) and 2-chloro-4,4- difluoro-spiro[5H-thieno[2,3-c]pyran-7,4'-piperidine] (31 1.72 mg, 1.1 1 mmol) in 1,2- dichloroethane (3 mL) is stirred at room temperature for 1 hr. and then sodium triacetoxyborohydride (429.41 mg, 2.03 mmol) is added. The reaction tube is sealed and stirred at room temperature for 18 hr. with the aid of a magnetic stirrer. Then, the reaction is quenched by addition of sodium bicarbonate saturated solution and the compound is extracted with ethyl acetate. The organic layer is separated, dried over magnesium sulfate and the solvent removed under reduced pressure. The compound is purified by supercritical fluid chromatography using AD-H as stationary phase to provide 230 mg (41%) of the title compound as white solid. MS (m/z): 548 (M+l).
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