HRID547301

反应详情

EQUATION

反应方程式

HRID 547301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under a nitrogen atmosphere 2-mercaptopyridine (1.23 g, 11.1 mmol) was added to a suspension of sodium hydride (0.41 g of 60%, 10 mmol) in DMF (30 mL). After hydrogen evolution had ceased, 1-[2-(3-chloropropoxy)ethyl]-2-propyl-1H-imidazo[4,5-c]quinolin-4-amine (3.20 g, 9.23 mmol) was added. After 2 hours analysis by HPLC indicated that starting material remained. 2-Mercaptopyridine (0.30 g) and sodium hydride (0.10 g) were added. After 3.5 hours the reaction mixture was poured into water with rapid stirring. The resulting brown solid was isolated by filtration and then triturated with diethyl ether to provide 3.71 g of 2-propyl-1-(2-{3-[(pyridin-2-yl)thio]propoxy}ethyl)-1H-imidazo[4,5-c]quinolin-4-amine as a solid.

WORKUP

后处理

  1. customThe resulting brown solid was isolated by filtration
  2. customtriturated with diethyl ether