반응식
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH:7]=[O:8].[Br:9]Br>C(Cl)(Cl)Cl>[Br:9][C:5]1[S:4][C:3]([CH:7]=[O:8])=[C:2]([CH3:1])[CH:6]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
A solution of 3-methyl-thiophene-2-carboxaldehyde (12.0 g) in chloroform (50 ml) was added drop-wise to bromine (5.1 ml) in chloroform over 30 minutes and then heated to 100° C. for 140 minutes. The reaction mixture was diluted with chloroform and washed with 10% aqueous sodium thiosulfate solution, saturated aqueous bicarbonate solution and water. The organic solution was dried over magnesium sulfate and concentrated. The product isolated after evaporation of the solvent was further purified by vacuum distillation (122° C., 4 mbar) to give the title compound as a green oil.
후처리
- washwashed with 10% aqueous sodium thiosulfate solution, saturated aqueous bicarbonate solution and water
- dry with materialThe organic solution was dried over magnesium sulfate
- concentrationconcentrated
- customThe product isolated
- customafter evaporation of the solvent
- distillationwas further purified by vacuum distillation (122° C., 4 mbar)
출처 및 근거
- ORD 기록
- ord-68d53e10beee4f048db9f744e8204245
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091237B2
연결된 노트
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