HRID1291348

反应详情

EQUATION

反应方程式

HRID 1291348 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-[4-(6-chloronicotinoyl]benzylthio]-3-methylthieno[3,2-d]pyrimidin-4(3H)-one (427 mg) and 4-piperidinopiperidine (202 mg) in pyridine (10 ml) was stirred at 80° C. for 10 hours. This reaction mixture was concentrated, the residue was dissolved in chloroform, and the solution was washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=50:1:0.1) and treated with HCl/ethyl acetate for conversion to hydrochloride to provide the title compound as colorless solid (373 mg).

WORKUP

后处理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in chloroform
  3. washthe solution was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=50:1:0.1)
  7. additiontreated with HCl/ethyl acetate for conversion to hydrochloride