反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[O:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([C:18](OCC)=[O:19])[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.CO.[Cl-].[NH4+]>C1(C)C=CC=CC=1.CCCCCC>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[O:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([CH:18]=[O:19])[CH2:14][CH2:13]2)=[CH:4][CH:3]=1参加物
7
反応条件
- 温度
- -68 °C
実験手順
3.03 g of ethyl 1-[2-bis(4-fluorophenyl)methoxyethyl]-4-piperidinecarboxylate (prepared as described in preparation 8) were dissolved in 30 ml of toluene, under a stream of nitrogen, and the resulting solution was cooled at -68° C. 8.2 ml of a 1M solution of diisobutylaluminum hydride in hexane was then added dropwise to the cooled mixture over a period of 10 minutes, and the mixture was stirred for 1 hour at -68° C. At the end of this time, 2 ml of methanol and 3 ml of a saturated aqueous solution of ammonium chloride were added to the reaction solution. The mixture was then extracted with ethyl acetate, to give 2.47 g (yield 91%) of the title compound as an oil, whose properties were the same as those of the product of step (a).
後処理
- extractionThe mixture was then extracted with ethyl acetate
出典と根拠
- ORDレコード
- ord-cbe09b54350b4e8787548fce94d652ef
- 出典データセット
- uspto-grants-1994_03
- 特許番号
- US05294623
関連ノート
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