HRID620168

反应详情

EQUATION

反应方程式

HRID 620168 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-chloromethyl-5-methyl-6-piperidino pyrimidine hydrochloride (4.63 g) and 2-mercapto-5-methoxybenzimidazole (3.18 g) in ethanol (180 ml) were heated at 50° for 5 hours. The solution was stripped to a residual glass, to which water was added, the pH raised to 13 (NaOH), and extracted with chloroform. Extracts were dried (K2CO3) and stripped to a residual glass which crystallised from ethyl acetate to give 5-methoxy-2-(5-methyl-6-piperidino-4-pyrimidinylmethylthio)-(1H)-benzimidazole, 5.67 g, m.p. 94°-96°.

WORKUP

后处理

  1. temperaturewere heated at 50° for 5 hours
  2. additionwas added
  3. extractionextracted with chloroform
  4. dry with materialExtracts were dried (K2CO3)
  5. customcrystallised from ethyl acetate