HRID32193

反应详情

EQUATION

反应方程式

HRID 32193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the 4-[5-methoxy-4-piperidin-1-yl-2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (88 mg, 0.17 mmol) produced in Example (72a), trifluoroacetic acid (0.25 mL, 3.2 mmol) and dichloromethane (0.5 mL) was stirred for 1 hour and 10 minutes at room temperature. Saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 56 mg of the title compound as a red solid.

WORKUP

后处理

  1. dry with materialThe separated organic layer was dried over anhydrous sodium sulfate
  2. filtrationThe desiccant was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane)