반응식
[C:1]([NH2:5])([CH3:4])([CH3:3])[CH3:2].[S:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[C:8]([S:15](Cl)(=[O:17])=[O:16])=[CH:7]1>O1CCCC1>[C:1]([NH:5][S:15]([C:8]1[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[S:6][CH:7]=1)(=[O:16])=[O:17])([CH3:4])([CH3:3])[CH3:2]참가 물질
4
실험 절차
To 25 g of tert-butyl amine in 100 ml of dry tetrahydrofuran was added dropwise with cooling 34 g of benzothiophene-3-sulfonyl chloride. The reaction mixture was allowed to come to room temperature and then poured into 200 g of ice. The phases were separated and the organic portion was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue thus obtained melted at 146°-148° after recrystallization from alcohol. It showed an absorption peak by NMR at 1.34 δ (singlet), for tert-butyl and 7.4-8.4 δ (multiplet) for benzothiophene consistent for the desired product.
후처리
- customto come to room temperature
- customThe phases were separated
- washthe organic portion was washed with water
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue thus obtained melted at 146°-148° after recrystallization from alcohol
출처 및 근거
- ORD 기록
- ord-c5dc0a21952943dbae1a78ce65def847
- 출처 데이터셋
- uspto-grants-1983_07
- 특허 번호
- US04391627
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