HRID253082

反应详情

EQUATION

反应方程式

HRID 253082 的结构方程式

PROCEDURE

实验过程

A solution of (−)-(3S,4R)-3-(3,5-bis-trifluoromethyl-benzyloxymethyl)-4-(4-fluoro-phenyl)-piperidine-1-carboxylic acid tert-butyl ester (1.10 g, 2.05 mmol) in a 1.25 M solution of hydrochloric acid in methanol (16.4 ml, 3.3 mmol) was stirred for 30 min. at 40° C. The reaction mixture was concentrated to dryness and the residue was partitioned between tert-butyl methyl ether and a 1 M aqueous sodium hydroxide solution. After extraction with three portions of tert-butyl methyl ether the combined organic layers were dried over sodium sulfate and concentrated in vacuo to 0.890 g (99.5%) of the title compound as a colorless white solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customthe residue was partitioned between tert-butyl methyl ether
  3. extractionAfter extraction with three portions of tert-butyl methyl ether the combined organic layers
  4. dry with materialwere dried over sodium sulfate
  5. concentrationconcentrated in vacuo to 0.890 g (99.5%) of the title compound as a colorless white solid