반응식
[CH3:1][O:2][C:3]([C:5]12[CH2:13][CH2:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[C:9]1=[N:8][N:7]([C:18]([NH:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=1)=[O:19])[CH2:6]2)=[O:4].C(N(CC)CC)C.Cl[S:39][N:40]([CH:46]([CH3:48])[CH3:47])[C:41](=[O:45])[O:42][CH2:43][CH3:44]>C(Cl)Cl>[CH3:1][O:2][C:3]([C:5]12[CH2:13][CH2:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[C:9]1=[N:8][N:7]([C:18]([N:20]([C:21]1[CH:22]=[CH:23][C:24]([C:27]([F:30])([F:28])[F:29])=[CH:25][CH:26]=1)[S:39][N:40]([CH:46]([CH3:48])[CH3:47])[C:41]([O:42][CH2:43][CH3:44])=[O:45])=[O:19])[CH2:6]2)=[O:4]참가 물질
5
반응물 3
생성물 1
시약·촉매·용매 1
실험 절차
To a solution of the title compound of Step B (2.0 g, 4.8 mmol) in 5 0 ml methylene chloride cooled to 0° C. was added triethylamine (1.0 g, 0.01 mol) and ethyl (chlorosulfenyl) (1-methylethyl)carbamate from Step D (1.4 g, 7.7 mmol). The mixture was allowed to warm to room temperature andstirred for one hour. The crude mixture was purified by silica column chromatography using ether-hexane (1:2) as eluent. The title compound (2.38 g) was obtained in about 90% purity (mp: 130°-134° ). Extraction of the product with ether-hexane (2:1) gave 1.8 g of highly pure material mp: 139°-140° C.
후처리
- customThe crude mixture was purified by silica column chromatography
출처 및 근거
- ORD 기록
- ord-b45f51290edc49b499deef29af23f2dc
- 출처 데이터셋
- uspto-grants-1996_02
- 특허 번호
- US05491162
연결된 노트
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