Dimethyl Sulfoxide → 2-Anilinothiazole-4-carbaldehyde
반응식
CS(C)=O.[NH:5]([C:12]1[S:13][CH:14]=[C:15]([CH2:17][OH:18])[N:16]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.C(N(CC)CC)C>O>[NH:5]([C:12]1[S:13][CH:14]=[C:15]([CH:17]=[O:18])[N:16]=1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1참가 물질
실험 절차
A dimethyl sulfoxide solution (120 ml) of 20 g of sulfur trioxide pyridine complex was added dropwise to a mixture comprising 8.3 g of 2-anilinothiazol-4-ylmethanol, 16.5 ml of triethylamine and 120 ml of dimethyl sulfoxide. The resulting mixture was stirred at room temperature for 10 minutes and then poured into water. followed by extraction with ethyl acetate. The extract was washed successively with aqueous acetic acid, aqueous sodium chloride solution and aqueous sodium hydrogen carbonate solution, and dried over anhydrous sodium sulfate. The residue afforded by evaporation of the solvent under reduced pressure was recrystallized from a mixture of benzene and acetone. The resulting product was a brown powder having the following physical properties.
후처리
- extractionfollowed by extraction with ethyl acetate
- washThe extract was washed successively with aqueous acetic acid, aqueous sodium chloride solution and aqueous sodium hydrogen carbonate solution
- dry with materialdried over anhydrous sodium sulfate
- customThe residue afforded by evaporation of the solvent under reduced pressure
- customwas recrystallized from a mixture of benzene and acetone
출처 및 근거
- ORD 기록
- ord-cec89db97521440fba29f14be0d6d555
- 출처 데이터셋
- uspto-grants-1990_06
- 특허 번호
- US04933355
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