HRID645484

反应详情

EQUATION

反应方程式

HRID 645484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of [1-(4-methoxy-benzyl)-4-phenylpiperidin-4-ylmethyl]carbamic acid tert-butyl ester (3.2 mmol) in CH2Cl2 is added 1-chloroethyl chloroformate (4.7 mmol), then the mixture is stirred at room temperature for 2.5 h. After the bulk of solvent is concentrated in vacuo, the residue suspended in ether and filtered. After the filtrate is concentrated in vacuo, the residue is suspended in hexane and filtered. The filtrate is concentrated in vacuo to give the 4-(tert-butoxycarbonylaminomethyl)-4-phenylpiperidine-1-carboxylic acid 1-chloroethyl ester, which is directly used for the next reaction without further purification.

WORKUP

后处理

  1. concentrationAfter the bulk of solvent is concentrated in vacuo
  2. filtrationfiltered
  3. concentrationAfter the filtrate is concentrated in vacuo
  4. filtrationfiltered
  5. concentrationThe filtrate is concentrated in vacuo