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CAS No. : | 337463-88-4 | MDL No. : | MFCD11101028 |
Formula : | C7H5BrN2O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | GDVHYNCHZKTTSQ-UHFFFAOYSA-N |
M.W : | 229.03 | Pubchem ID : | 21873772 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | Step 4 To a solution of Compound (9) (3.12 g, 13.7 mmol) in tetrahydrofuran (50 mL), borane-tetrahydrofuran complex (33 mL, 33.0 mmol) was added at room temperature. The solution was then stirred at 90C for 1.5 hours. Methanol (2.0 mL) was added to the reaction solution, and then the mixture was stirred at 90C for 20 minutes. The reaction solution was concentrated in vacuo. The residue was dissolved in ethyl acetate, washed with aqueous saturated sodium bicarbonate, dried with anhydrous magnesium sulfate, and then concentrated in vacuo to yield subject compound (10) (3.17 g, 100%) as a yellow powder.1H-NMR (DMSO-d6) 57.04 (1H, br s), 6.69 (1H, d, J = 7.8 Hz), 6.40 (1H, d, J = 7.8 Hz), 3.91 (2H, t, J = 4.2Hz), 3.19-3.23 (2H, m) LC/MS (Method A): 1.44 min, [M+H]+ = 215.2. | |
99% | With diborane; In tetrahydrofuran; for 1h;Cooling with ice; Reflux; | Under ice bath conditions, Borane in tetrahydrofuran (5.5 mL, 5.5 mmol, 1.0 M) Add dropwise to compound 3.2 (500 mg, 2.19 mmol) In a solution of tetrahydrofuran (25 mL), The reaction system was stirred under reflux with heating for 1 hour. The reaction was then carefully quenched with methanol (10 drops) under reflux. The mixture was cooled to room temperature and concentrated under reduced pressure to remove solvent. The residue was chromatographed on silica gel ( petroleum ether / ethyl acetate = 5/1) Purification afforded compound 23.1 (470 mg, yield: 99%) It is a white solid. |
87% | With dimethylsulfide borane complex; potassium carbonate; In tetrahydrofuran; at 70℃; for 0.25h;Inert atmosphere; | Part IV- Synthesis of 6-Bromo-3,4-dihydro-2H-pyrido[3,2-b] [1,4]oxazine; 6-Bromo-4H-pyrido[3,2-b][1,4]oxazin-3-one (1.35 g, 5.89 mmol) was dissolved inTHF (40 mL). Boranedimethylsulphide complex (2.0 Min THF, 5.89 mL, 11.79 mmol) wasadded and the resulting mixture heated to 70 C under nitrogen for 15 minutes. Next, thereaction mixture was cooled to room temperature, quenched with methanol ( ~5 mL ), and then dried under vacuum to obtain a white solid. The crude material was dissolved indichloromethane and washed with H20. The aqueous phase was discarded and the organicphase was dried under vacuum to give 6-bromo-3,4-dihydro-2H-pyrido[3,2-b ][1,4]oxazine.Yield: 1.1 g (87%). LCMS (ESI): calc. C7H7BrN20 = 214, 216; obs. M+H = 215, 217. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | With copper(l) iodide; potassium carbonate; N,N`-dimethylethylenediamine; In 1,4-dioxane; at 100℃; | Compound 3.2 (1.9 g, 8.29 mmol),<strong>[955368-90-8]2-allyl-6-(methylthio)-1H-pyrazolo[3,4-d]pyrimidin-3(2H)-one</strong> (1.84 g, 8.29 mmol),Cuprous iodide (1.5 g, 8.29 mmol),Anhydrous potassium carbonate (2.35 g, 17 mmol)And N,N-dimethylethylenediamine (0.73g, 8.29mmol)Add to 1,4-dioxane (30 mL),The reaction system was stirred at 100 C overnight.Cool to room temperature,Filter the reaction solution,The filtrate is concentrated,The residue was purified by silica gel column chromatography (EtOAc /EtOAcCompound 3-1 (1.56 g, yield: 51%) was obtained as a yellow solid. |
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