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[ CAS No. 13139-17-8 ] {[proInfo.proName]}

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Chemical Structure| 13139-17-8
Chemical Structure| 13139-17-8
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Product Details of [ 13139-17-8 ]

CAS No. :13139-17-8 MDL No. :MFCD00005513
Formula : C12H11NO5 Boiling Point : -
Linear Structure Formula :C7H7CO2NC2O2C2H4O InChI Key :MJSHDCCLFGOEIK-UHFFFAOYSA-N
M.W : 249.22 Pubchem ID :83172
Synonyms :

Safety of [ 13139-17-8 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P280-P305+P351+P338 UN#:N/A
Hazard Statements:H302-H315-H319-H332-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 13139-17-8 ]

* 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 [ 13139-17-8 ]

[ 13139-17-8 ] Synthesis Path-Downstream   1~12

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  • [ 13139-17-8 ]
  • [ 23356-96-9 ]
  • [ 6216-63-3 ]
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  • [ 103639-57-2 ]
  • [ 190967-63-6 ]
  • 3
  • [ 13139-17-8 ]
  • [ 4378-19-2 ]
  • [ 137584-40-8 ]
YieldReaction ConditionsOperation in experiment
45 g With sodium carbonate; In tetrahydrofuran; water; at 20℃; for 16h; Step 1. To a mixture of aq Na2C03 (82 g, 0.78 mol) and compound 73-1 (20 g, 0.19 mol) was added Cbz-OSu (57 g, 0.23 mol) in THF (150 mL). After the mixture was stirred at r.t. for 16 h, it was adjusted to pH > 10 and the solution was extracted with EtOAc (400 mL x 2). The aqueous layer was acidified to pH < 1 with conc.HCl and the solution was extracted with EtOAc (500 mL x 2). The organic layers were dried over Na2S04 and concentrated to give compound 73-2 (45 g, 0.19 mol), which was used for next step without further purification.
  • 4
  • [ 13139-17-8 ]
  • [ 54288-70-9 ]
  • [ 166953-64-6 ]
YieldReaction ConditionsOperation in experiment
98% With 4-methyl-morpholine; dmap; at 20℃; for 16h; To a solution of <strong>[54288-70-9]4-bromopiperidine hydrobromide</strong> (3.0 g, 12.2 mmol) in tetrahydrofuran (30 ml) were added 1-[(benzyloxy)carbonyl]oxy}-2,5-pyrrolidinedione (3.20 g, 12.9 mmol), N-methylmorpholine (1.62 ml, 14.7 mmol) and 4-N,N-dimethylaminopyridine (30 mg) at room temperature, and stirred at room temperature for 16 hours. The reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with a 1N-aqueous hydrochloric acid solution, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent, and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate = 1/1) to obtain benzyl 4-bromo-1-piperidinecarboxylate (3.58 g, 98percent).
  • 5
  • [ 13139-17-8 ]
  • [ 30482-25-8 ]
  • [ 869895-16-9 ]
YieldReaction ConditionsOperation in experiment
In dichloromethane; at 20℃; for 1.0h; To a solution of 28 (1.07 g, 6.28 mmol) in CH2Cl2 (60 mL), was added N-(benzyloxycarbonyloxy)succinimide (1.72 g, 6.91 mmol). The reaction mixture stirred at room temperature for approximately one hour before most of the solvent was removed (55 mL) in vacuo. The crude product was purified by a silica gel chromatography (8percent-12percent MeOH/CH2Cl2) to give benzyl 1,4-dioxaspiro[4.5]dec-8-ylmethylcarbamate. LCMS (ES) m/z 306.2 (M+H)+.
  • 6
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  • diisopropylethylamine (DIPEA) [ No CAS ]
  • [ 18650-39-0 ]
  • [ 60369-19-9 ]
YieldReaction ConditionsOperation in experiment
100% In dichloromethane (DCM); hexane; ethyl acetate; Method A (S)-Piperidine-1,2-dicarboxylic acid 1-benzyl ester 2-methyl ester To a stirred suspension of <strong>[18650-39-0](S)-piperidine-2-carboxylic acid methyl ester hydrochloride</strong> salt (5.0 g, 27.8 mmol) in dichloromethane (DCM) (35 mL) at 0° C. was added diisopropylethylamine (DIPEA) (10.1 mL, 58.4 mmol) followed by N-(benzyloxycarbonyloxy) succinimide (7.63 g, 30.6 mmol). The reaction mixture was allowed to warm to room temperature and stirred overnight. The residue was diluted with DCM and washed with 1.0-M HCl. The organic layer was washed with brine, dried(Na2SO4), filtered and concentrated in vacuo. The residue was purified by flash chromatography (20percent ethyl acetate in hexane) to afford the title compound as a pale yellow oil (7.72, 100percent): 1H NMR (400 MHz, CD3OD) delta 1.19-1.88 (5 H, m), 2.15-2.28 (1H, m), 2.91-3.12 (1H, m), 3.70-3.73 (3H, 2s), 4.00-4.07 (1H, m), 4.82-4.87 (1H, m), 5.03-5.21 (2H, m), 7.24-7.39 (5H, m); 13C NMR (100 MHz, CD3OD) delta 22.0, 22.1 (CH2), 26.0, 26.1 (CH2), 28.1 (CH2), 43.4, 43.5 (CH2), 53.1 (CH3), 56.2, 56.5 (CH), 68.8, 68.9 (CH2), 129.2 (CH), 129.5 (CH), 129.9 (CH), 138.4 (C), 167.0 (CO), 173.7 (CO).
  • 7
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  • [ 183673-71-4 ]
  • [ 288154-16-5 ]
YieldReaction ConditionsOperation in experiment
With aq. sodium hydroxide; In 1,2-dimethoxyethane; aqueous sodium hydroxide; (a) Allyl 4-benzyloxycarbonylaminopiperidine-4-carboxylate. 4-Amino-1-tert-butoxycarbonylpiperidine-4-carboxylic acid (18.0 g) was dissolved in 0.03M aqueous sodium hydroxide (750 mL), and 1,2-dimethoxyethane (100 mL). The pH was adjusted to 9.5 with dilute hydrochloric acid, and the suspension was added to an ice-cold solution of N-(benzyloxycarbonyloxy)succinimide (28.8 g) in 1,2-dimethoxyethane (100 mL). The pH was kept at 9.5 by addition of aq. sodium hydroxide, and the mixture was stirred at room temperature. More N-(benzyloxycarbonyloxy)succinimide (3 g) was added after 7 h, then stirring continued overnight. After evaporation to remove the 1,2-dimethoxyethane, the aqueus residue was extracted with ether then acidified to pH 4 and extracted with ethyl acetate. This extract was washed with dilute hydrochloric acid, water and brine, dried and evaporated. Trituration of the oily residue gave 4-benzyloxycarbonylamino-1-tert-butoxycarbonylpiperidine-4-carboxylic acid (23 g).
In sodium hydroxide; 1,2-dimethoxyethane; (a) Methyl 4-benzyloxycarbonylamino-1-tert-butoxycarbonylpiperidine-4-carboxylate. 4-Amino-1-tert-butoxycarbonylpiperidine-4-carboxylic acid (18.0 g) was dissolved in 0.03M aqueous sodium hydroxide (750 ml), and 1,2-dimethoxyethanol (DME, 100 ml). The pH was adjusted to 9.5 with dilute hydrochloric acid, and the suspension was added to an ice-cold solution of N-(benzyloxycarbonyloxy)succinimide (28.8 g) in DME (100 ml). The pH was kept at 9.5 by addition of aqueous sodium hydroxide, and the mixture was stirred at room temperature. More N-(benzyloxycarbonyloxy)succinimide (3 g) was added after 7 hours, then stirring was continued overnight. After evaporation, the aqueous residue was extracted with ether then acidified to pH4 and extracted with ethyl acetate. This extract was washed with dilute hydrochloric acid, water and brine, dried and evaporated. Trituration of the oily residue gave 4-benzyloxycarbonylamino-1-tert-butoxycarbonylpiperidine-4-carboxylic acid (23 g).
  • 8
  • [ 13139-17-8 ]
  • [ 15099-85-1 ]
  • [ 26250-86-2 ]
  • 9
  • [ 13139-17-8 ]
  • [ 625-05-8 ]
  • [ 51219-55-7 ]
YieldReaction ConditionsOperation in experiment
65.7% With sodium hydroxide; In tetrahydrofuran; methanol; water; at 0 - 20℃; for 17.5h; N-(Benzyloxycarbonyloxy)succinimide (24.4 g, 1 equiv, 98 mmol) was added to a solution of <strong>[625-05-8]3-amino-3-methylbutanoic acid</strong> (16.0 g, 97.2 mmol) in methanol and water (200 mL: 100 mL) followed by the addition of THF (100 mL) to give a clear solution. <n="86"/>The solution was cooled in an ice bath for 15 min and a solution of 5 N sodium hydroxide (39 mL, 2 equiv) was added over 15 min. The solution was stirred at 0 0C for an additional hour and stirred at RT for 17 h. The organic solvent was removed and the aqueous was extracted with ethyl acetate (2x 200 mL). The aqueous layer was acidified with 6 N HCl (50 mL) and extracted with ethyl acetate (4x 200 mL). The organic layer was dried over anh. MgSO4, filtered, and concentrated to an orange yellow oil (16.2 g, 65.7percent). This oil was used without further purification. LRMS (ESI -ve) for Ci3H17NO4 (251.1); found: 250.
  • 10
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  • [ 24629-25-2 ]
  • [ 6216-62-2 ]
  • 11
  • [ 2762-32-5 ]
  • [ 13139-17-8 ]
  • [ 58632-95-4 ]
  • [ 149057-19-2 ]
YieldReaction ConditionsOperation in experiment
80% 54a. 4-((Benzyloxy)carbonyl)-1 -(tert-butoxycarbonyl)piperazine-2- carboxylic acidThe tile compound was prepared according to the procedure of [Kempf, D. J.; Norbeck, D. W.; Sham, H. L U.S. Patent 5,455,351 , Oct 3, 1995]. Piperazine-2-carboxylic acid (10.0 g, 77.0 mmol) was dissolved in a 1 :1 solution of 1 ,4-dioxane:water (100 mL) at room temperature with vigorous stirring. The clear solution was adjusted to pH 11 by the addition of an aqueous solution of sodium hydroxide (80 mL of a 1Lambda/ solution). The pH was monitored in situ with a pH meter throughout the reaction. The reaction flask was fitted with an addition funnel that contained a solution of Lambda/-alpha- (benzyloxycarbonyloxy) succinamide (13.6 g, 55 mmol) in 1 ,4-dioxane (50 mL). The Lambda/-alpha-(benzyloxycarbonyloxy) succinamide solution was added over 45 minutes at room temperature and the pH was kept above 10 by the periodic addition of 1 Lambda/ sodium hydroxide. The pH of the solution was adjusted to 9.5 and 2-(teAf-butoxycarbonyloxyimino)-2-phenylacetonitrile (13.4 g, 55 mmol) was added as a solution in 1 ,4-dioxane (50 mL) over 10 minutes. The pH was maintained at 9.5 and the solution was stirred at room temperature for 17 hours. The solution was then acidified to pH 2 and the aqueous solution was washed with diethyl ether (3 x 150 mL). The aqueous solution was cooled to O0C and acidified by adding of concentrated hydrochloric acid. The acidic solution was extracted with ethyl acetate (5 x 150 mL). The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo. The residue was triturated with a 1 :1 solution of dichloromethane: hexanes (150 mL) and the solvent was removed in vacuo to provide the product as a viscous yellow oil (15.7 g, 43 mmol, 80%). Rf = 0.60 (66:34 dichloromethane: ethyl acetate + 0.1% (v/v acetic acid); 1H-NMR (400 MHz, DMSO) delta 13.0 (br s, 1 H), 7.37-7.36 (m, 5H), 5.05 (s, 2H), 4.54-4.33 (m, 2H), 3.90-3.66 (m, 2H), 3.07-2.81 (m, 4H), 1.38 (s, 9H); Mass spectrum (ESI +ve) m/z 365.1 (MH+).
  • 12
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  • [ 2491-18-1 ]
  • [ 56762-93-7 ]
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