Aluminium lithium hydride → N-methyl-3-(m-trifluoromethylphenyl)-piperidine
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]([F:24])([F:23])[C:9]1[CH:10]=[C:11]([CH:15]2[CH2:20][CH2:19][CH2:18][N:17]([CH:21]=O)[CH2:16]2)[CH:12]=[CH:13][CH:14]=1>O1CCCC1>[CH3:21][N:17]1[CH2:18][CH2:19][CH2:20][CH:15]([C:11]2[CH:12]=[CH:13][CH:14]=[C:9]([C:8]([F:7])([F:23])[F:24])[CH:10]=2)[CH2:16]1参加物
4
反応条件
- 温度
- 7 °C
実験手順
2 g of lithium aluminum hydride were added in small amounts to 100 ml of tetrahydrofuran and the mixture was cooled to 7° C. A solution of 10 g of the product of Step A in 60 ml of tetrahydrofuran was added thereto over about 20 minutes while keeping the temperature at 5° to 10° C. and the mixture was stirred for an hour at room temperature and was then poured into ice. The mixture was stirred for 15 minutes at room temperature and was then filtered. The filtrate was extracted with ethyl acetate and the organic phase was washed with aqueous sodium chloride solution, dried over magnesium sulfate and evaporated to dryness to obtain 9.1 g of N-methyl-3-(m-trifluoromethylphenyl)-piperidine in the form of a resin.