반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]([OH:9])=[O:8])=[C:4]([Si:10]([CH3:13])([CH3:12])[CH3:11])[CH:3]=1.S(Cl)([Cl:16])=O.Cl.[CH:19]([NH:22][OH:23])([CH3:21])[CH3:20].C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[Cl:1][C:2]1[S:6][C:5]([C:7]([Cl:16])=[O:8])=[C:4]([Si:10]([CH3:13])([CH3:12])[CH3:11])[CH:3]=1.[Cl:1][C:2]1[S:6][C:5]([C:7]([N:22]([OH:23])[CH:19]([CH3:21])[CH3:20])=[O:9])=[C:4]([Si:10]([CH3:13])([CH3:12])[CH3:11])[CH:3]=1참가 물질
8
반응물 4
생성물 2
시약·촉매·용매 2
실험 절차
5-Chloro-3-(trimethylsilyl)-2-thiophenecarboxylic acid chloride was prepared by the reaction of 1 g 5-chloro-3-(trimethylsilyl)-2-thiophenecarboxylic acid (prepared as in Example 263) and 6 mL thionyl chloride, using the procedure of step a in Example 248. This product was dissolved in CH2Cl2 at 0° C. and added to a mixture of N-isopropylhydroxylamine hydrochloride (0.55 g, 5 mmol) and 4 g NaHCO3 in 20 mL CH2Cl2 and 20 mL water. The resulting reaction mixture was stirred at RT for additional 3 h. The organic layer was separated, washed with brine, dried and concentrated. The residue was purified by flash chromatography with 8% ethyl acetate/hexane to give 80 mg of the title compound. m.p. 146°-150° C.
후처리
- customThe resulting reaction mixture
- customThe organic layer was separated
- washwashed with brine
- customdried
- concentrationconcentrated
- customThe residue was purified by flash chromatography with 8% ethyl acetate/hexane
출처 및 근거
- ORD 기록
- ord-d9dab582b1f3417fbf7803c2a24a8d1d
- 출처 데이터셋
- uspto-grants-1998_01
- 특허 번호
- US05705513
연결된 노트
불러오는 중…