반응식
[Br:1][C:2]1[CH:23]=[CH:22][C:5]([C:6]([N:8]2[CH2:13][CH2:12][C:11]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3O)([OH:14])[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.C(=O)([O-])[O-:25].[K+].[K+].O.[CH2:31]([O:33][C:34](=[O:39])[C:35](Br)([CH3:37])[CH3:36])[CH3:32]>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([N:8]2[CH2:13][CH2:12][C:11]([C:15]3[CH:16]=[C:17]([CH:18]=[CH:19][CH:20]=3)[O:25][C:35]([CH3:37])([CH3:36])[C:34]([O:33][CH2:31][CH3:32])=[O:39])([OH:14])[CH2:10][CH2:9]2)=[O:7])=[CH:22][CH:23]=1참가 물질
5
실험 절차
801 mg of {1-(4-bromobenzoyl)-4-(2-hydroxyphenyl)-4-hydroxypiperidine was stirred for 9 hours at the ambient temperature of 100° C. in the presence of 1.20 g (8.68 mmol) of potassium carbonate in 4.00 g (20.5 ml) of ethylα-bromoisobutyrate. After completion of the reaction, The reaction mixture was cooled, and water was added thereto, followed by extraction with chloroform. Subsequently, the extract was dried over anhydrous sodium sulfate. Chloroform and the remained ethyl α-bromoisobutyrate was distilled off under reduced pressure to obtain 902 mg (86.4%) of ethyl 3-{1-(4-bromobenzoyl)-4-hydroxypiperidin-4-yl}α,α-dimethylphenoxyacetate.
후처리
- customAfter completion of the reaction
- temperatureThe reaction mixture was cooled
- extractionfollowed by extraction with chloroform
- dry with materialSubsequently, the extract was dried over anhydrous sodium sulfate
- distillationChloroform and the remained ethyl α-bromoisobutyrate was distilled off under reduced pressure
출처 및 근거
- ORD 기록
- ord-004d54879f88431ca2eb482dd4019232
- 출처 데이터셋
- uspto-grants-1995_05
- 특허 번호
- US05411972
연결된 노트
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