HRID1689882

反应详情

EQUATION

反应方程式

HRID 1689882 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-bromo-2,N-dimethyl-propionamide (312 mg), 1-BOC-piperazine (323 mg) and silver oxide (800 mg) was stirred in toluene (5 mL) at reflux. After 24 h the reaction mixture was cooled, filtered through celite, diluted with chloroform, washed with brine, dried (MgSO4) and the solvent was removed in vacuo to yield 4-(1-methyl-1-methylcarbamoyl-ethyl)-piperazine-1-carboxylic acid tert-butyl ester (461 mg). Removal of the BOC group with HCl yielded the desired compound, which was isolated as the hydrochloride salt.

WORKUP

后处理

  1. temperatureat reflux
  2. temperatureAfter 24 h the reaction mixture was cooled
  3. filtrationfiltered through celite
  4. additiondiluted with chloroform
  5. washwashed with brine
  6. dry with materialdried (MgSO4)
  7. customthe solvent was removed in vacuo