반응식
[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]#[CH:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH3:22]I.O>CN(C)C=O.CCCCCC>[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[N:9]([CH3:18])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]#[C:17][CH3:22])[C:6]=2[CH:5]=[CH:4][CH:3]=1참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
2.72 g (10 mmol) of 7-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one was dissolved in 20 ml of N,N-dimethylformamide. 1.31 g (30 mmol) of sodium hydride dispersion (55% in oil) was washed with n-hexane and then introduced at room temperature into the above solution. After 10 minutes 0.95 ml (15 mmol) of methyl iodide was added thereto and the mixture was stirred at room temperature for a further 3 hours. The reaction mixture was poured into 300 ml of water and extracted four times with methylene chloride. The organic extracts were washed four times with water and dried over magnesium sulphate. After chromatography of the residue on silica gel while eluting with ethyl acetate and recrystallization from ethyl acetate, there was obtained 7-chloro-4,5-dihydro-5-methyl-3-(1-propynyl)-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 243°-244°.
후처리
- additionintroduced at room temperature into the above solution
- extractionextracted four times with methylene chloride
- washThe organic extracts were washed four times with water
- dry with materialdried over magnesium sulphate
- washAfter chromatography of the residue on silica gel while eluting with ethyl acetate and recrystallization from ethyl acetate
출처 및 근거
- ORD 기록
- ord-bb3fce22e4004d98aed4c110664b2afe
- 출처 데이터셋
- uspto-grants-1989_09
- 특허 번호
- US04863920
연결된 노트
불러오는 중…