반응식
[CH2:1]([C:3]1[C:23]([NH2:24])=[C:6]2[C:7]([O:21][CH3:22])=[CH:8][CH:9]=[C:10]([C:11]3[C:16]([CH3:17])=[CH:15][C:14]([CH3:18])=[CH:13][C:12]=3[O:19][CH3:20])[N:5]2[N:4]=1)[CH3:2].[CH3:25][CH2:26][C:27](=O)[CH2:28][CH3:29].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>C(O)(=O)C>[CH2:1]([C:3]1[C:23]([NH:24][CH:27]([CH2:28][CH3:29])[CH2:26][CH3:25])=[C:6]2[C:7]([O:21][CH3:22])=[CH:8][CH:9]=[C:10]([C:11]3[C:16]([CH3:17])=[CH:15][C:14]([CH3:18])=[CH:13][C:12]=3[O:19][CH3:20])[N:5]2[N:4]=1)[CH3:2]참가 물질
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
To a solution of 2-ethyl-4-methoxy-7-(2-methoxy-4,6-dimethylphenyl)pyrazolo[1,5-a]pyridin-3-amine (100 mg) in acetic acid (10 mL) there was added 3-pentanone (0.04 mL), and then sodium triacetoxyborohydride (85.0 mg) was slowly added at room temperature and the mixture was stirred for 3 hours. A 5 N aqueous sodium hydroxide solution was added while cooling on ice, and then extraction was performed with ethyl acetate, the organic layer was washed with saturated aqueous sodium hydrogencarbonate and brine and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was subjected to silica gel column chromatography (10 g), and the title compound (69 mg) was obtained from the n-hexane:ethyl acetate (5:1) fraction as yellow crystals.
후처리
- temperaturewhile cooling on ice
- extractionextraction
- washthe organic layer was washed with saturated aqueous sodium hydrogencarbonate and brine
- dry with materialdried over magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
출처 및 근거
- ORD 기록
- ord-bf2e18615a834fdc9d01496b0f8b0599
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091215B2
연결된 노트
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