반응식
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[C:11]([CH:14]=[O:15])[S:12][CH:13]=2)=[CH:5][CH:4]=1.CC(=CC)C.Cl([O-])=[O:24].[Na+].P([O-])(O)(O)=O.[Na+]>O.C(O)(C)(C)C>[F:17][C:2]([F:16])([F:1])[C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:10]=[C:11]([C:14]([OH:24])=[O:15])[S:12][CH:13]=2)=[CH:7][CH:8]=1참가 물질
실험 절차
A solution of 4-[4-(trifluoromethyl)phenyl]thiophene-2-carbaldehyde (intermediate 37, 1.23 g), t-butanol (20 ml) and 2-methyl-2-butene (10 ml) was cooled to 0° C. To this was added drop-wise, a solution of sodium chlorite (3.8 g) and sodium dihydrogen phosphate (4.03 g) in water (15 ml). After the addition was complete, the mixture was allowed to warm to room temperature and was stirred for 4 hours. The solution was then concentrated and partitioned between water and ethyl acetate. The aqueous layer was washed with a second ethyl acetate portion and the organic liquors were combined, washed with brine, then dried (MgSO4). The solution was then absorbed onto silica and loaded onto a SPE (Si) cartridge. The product was eluted with neat ethyl acetate to afford the title compound as a white solid.
후처리
- additionTo this was added drop-wise
- additionAfter the addition
- concentrationThe solution was then concentrated
- custompartitioned between water and ethyl acetate
- washThe aqueous layer was washed with a second ethyl acetate portion
- washwashed with brine
- dry with materialdried (MgSO4)
- customThe solution was then absorbed onto silica
- washThe product was eluted with neat ethyl acetate
출처 및 근거
- ORD 기록
- ord-6f39bd3263d74268b672227e11e8ee23
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091237B2
연결된 노트
불러오는 중…