HRID556953

反应详情

EQUATION

反应方程式

HRID 556953 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a chilled solution of 4-(4-chloro-phenyl)-piperidine-1,4-dicarboxylic acid 1-tert-butyl ester 4-methyl ester (700 mg, 1.98 mmol) in 6 ml ether was added dropwise 2 ml lithium aluminium hydride 1M solution in ether. The reaction was stirred at 0° C. for 3 hours, then water (100 ml) was slowly added. The resulting gel was filtered and the aqueous filtrate was extracted three times with ether. The combined organic layers were dried with magnesium sulfate and concentrated under vacuum. Recovered oil was purified by silica gel chromatography, eluting with hexane-ethyl acetate (6:4) to give the title compound (297 mg, 46%).

WORKUP

后处理

  1. filtrationThe resulting gel was filtered
  2. extractionthe aqueous filtrate was extracted three times with ether
  3. dry with materialThe combined organic layers were dried with magnesium sulfate
  4. concentrationconcentrated under vacuum
  5. customRecovered oil
  6. customwas purified by silica gel chromatography
  7. washeluting with hexane-ethyl acetate (6:4)