반응식
[OH:1][N:2]=[C:3]1[S:7][C:6](=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:9]#[N:10])[CH:5]=[CH:4]1.C(N(CC)CC)C.[CH3:24][S:25](Cl)(=[O:27])=[O:26].O>C1COCC1>[CH3:24][S:25]([O:1][N:2]=[C:3]1[S:7][C:6](=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:9]#[N:10])[CH:5]=[CH:4]1)(=[O:27])=[O:26]참가 물질
실험 절차
5 g (22 mmol) of (5-Hydroxyimino-5H-thiophen-2-ylidene)-phenyl-acetonitrile are dissolved in 50 ml of THF and cooled in an ice bath. After adding 4.6 ml (33 mmol) of triethylamine to the solution, 1.9 ml (24 mmol) of methanesulfonyl chloride are added dropwise, keeping the temperature below 5° C. The reaction mixture is stirred while cooling in an ice bath for 30 min. The reaction mixture is poured into 200 ml of water, and extracted with ethyl acetate. The organic phase is washed with hydrochloric acid solution and sodium chloride solution. The organic phase is dried over MgSO4, the solvent is distilled off, and the residue is purified by recrystallization from toluene. 5.2 g (77%) of (5-Methylsulfonyloxyimino-5H-thiophen-2-ylidene)-phenyl-acetonitrile are obtained in the form of greenish brown crystals having a melting point of 160-162° C. (dec.).
후처리
- temperaturecooled in an ice bath
- additionare added dropwise
- customthe temperature below 5° C
- temperaturewhile cooling in an ice bath for 30 min
- extractionextracted with ethyl acetate
- washThe organic phase is washed with hydrochloric acid solution and sodium chloride solution
- dry with materialThe organic phase is dried over MgSO4
- distillationthe solvent is distilled off
- customthe residue is purified by recrystallization from toluene
출처 및 근거
- ORD 기록
- ord-607654a676584d24bb1028defa5a2427
- 출처 데이터셋
- uspto-grants-1999_12
- 특허 번호
- US06004724
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