반응식
C[Li].[CH2:3]([O:10][C:11]1[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=1)[C:14]([OH:16])=O)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.O1CCC[CH2:21]1.O>CCOCC>[CH3:21][C:14]([C:13]1[CH:17]=[CH:18][CH:19]=[C:11]([O:10][CH2:3][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:12]=1)=[O:16]참가 물질
6
실험 절차
Over a period of 1.5 hours, methyl lithium (531 ml. of a 2 molar solution, 1.06 M) is added under a nitrogen atmosphere to a rapidly stirring solution of 3-benzyloxybenzoic acid (116 g., 0.532 M) in ether (250 ml.) - tetrahydrofuran (1400 ml.) maintained at 15°-20° C. After stirring an additional 0.75 hour at 10°-15° C., water (600 ml.) is slowly added keeping the reaction temperature below 20° C. The aqueous layer is separated and extracted with ether (3×250 ml.). The organic phases are combined, washed with saturated sodium chloride solution (4×300 ml.), dried over sodium sulfate, and concentrated under vacuum to give the product as an oil.
후처리
- temperaturemaintained at 15°-20° C
- customthe reaction temperature below 20° C
- customThe aqueous layer is separated
- extractionextracted with ether (3×250 ml.)
- washwashed with saturated sodium chloride solution (4×300 ml.)
- dry with materialdried over sodium sulfate
- concentrationconcentrated under vacuum
출처 및 근거
- ORD 기록
- ord-e8f37ef5ddf946cea6c954ee30c4ea29
- 출처 데이터셋
- uspto-grants-1979_08
- 특허 번호
- US04165323
연결된 노트
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