(Chlorothio)formyl chloride → 5-(4-Chloro-2-methoxyphenyl)-1,3,4-oxathiazol-2-one
반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[C:4]([O:11][CH3:12])[CH:3]=1.Cl[C:14]([S:16]Cl)=[O:15]>O1CCCC1>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]2[O:7][C:14](=[O:15])[S:16][N:8]=2)=[C:4]([O:11][CH3:12])[CH:3]=1참가 물질
4
실험 절차
In tetrahydrofuran (100 ml), 4-chloro-2-methoxybenzamide (5.67 g, 30.5 mmol) prepared in the Step 7-1-1 and chlorocarbonylsulfenyl chloride (4.40 g, 33.6 mmol) were suspended, and the mixture was heated under reflux for 1.5 hours. After being allowed to cool, the mixture was subjected to extraction with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (n-hexane:ethyl acetate=7:1) to give the title compound (5.33 g, 71%).
후처리
- temperaturethe mixture was heated
- temperatureunder reflux for 1.5 hours
- temperatureto cool
- extractionthe mixture was subjected to extraction with ethyl acetate
- dry with materialthe extract was dried over anhydrous magnesium sulfate
- concentrationconcentrated
- customThe concentrate was purified by silica gel column chromatography (n-hexane:ethyl acetate=7:1)
출처 및 근거
- ORD 기록
- ord-bbbecceb172e405d9d3af1c5778f1aaa
- 출처 데이터셋
- uspto-grants-2015_12
- 특허 번호
- US09200008B2
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