Water → HCID 21471776, 화합물
반응식
[Cl:1][CH2:2][C:3]([C:5]1[S:15][C:8]2[C:9](=[O:14])[NH:10][CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=1)=O.O>C([SiH](CC)CC)C.FC(F)(F)C(O)=O>[Cl:1][CH2:2][CH2:3][C:5]1[S:15][C:8]2[C:9](=[O:14])[NH:10][CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=1참가 물질
5
반응 조건
- 온도
- 50 °C
실험 절차
A mixture of 1.9 g of 2-chloroacetyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one in 5.4 ml of triethylsilane and 15 ml of trifluoroacetic acid was stirred at 50° C. for 12 hours. The mixture was poured into water, alkalified and extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was purified by column chromatography on a silica gel to give 0.85 g of 2-chloroethyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one as white crystals, m.p. 156°-158° C.
후처리
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- customdried
- concentrationconcentrated
- customThe residue was purified by column chromatography on a silica gel
출처 및 근거
- ORD 기록
- ord-4d15ec676cfb411ea4a37f98e9ecc9d9
- 출처 데이터셋
- uspto-grants-1996_07
- 특허 번호
- US05532240
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