HRID128216

反应详情

EQUATION

反应方程式

HRID 128216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
7 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. additionwas then poured into ice
  2. stirringThe mixture was stirred for 15 minutes at room temperature
  3. filtrationwas then filtered
  4. extractionThe filtrate was extracted with ethyl acetate
  5. washthe organic phase was washed with aqueous sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. customevaporated to dryness