反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
To 2.04 g of a 5% palladium-carbon catalyst, 15 ml of water containing 10.2 g of potassium acetate was added. Then, a solution of 10.18 g (21.6 mmol) of 4-chloro-6-[(2-ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridin-3-yl)methyl]-2-(nitrophenyl)quinoline obtained in Example 4 dissolved in 30 ml of ethyl acetate and 240 ml of ethanol at 70° C. was added thereto, and the thus-prepared mixture was stirred under a hydrogen atmosphere at 60° C. for 3 hours. After adding 150 ml of chloroform and 200 ml of water thereto, the thus-prepared mixture was filtered through celite. The resulting filtrate was separated out, and the organic layer obtained was concentrated to 95.0 g in an evaporator. After allowing to stand at 0° C., the crystals precipitated were collected by filtration. The resulting filtration residue was washed with 10 ml of ethanol three times and dried under reduced pressure at 40° C. to obtain 6.70 g of 2-{6-[(2-ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridin-3-yl)methyl]quinolin-2-yl}aniline.
WORKUP
后处理
- filtrationthe thus-prepared mixture was filtered through celite
- customThe resulting filtrate was separated out
- customthe organic layer obtained
- concentrationwas concentrated to 95.0 g in an evaporator
- customto stand at 0° C.
- customthe crystals precipitated
- filtrationwere collected by filtration
- filtrationThe resulting filtration residue
- washwas washed with 10 ml of ethanol three times
- customdried under reduced pressure at 40° C.