反応 #5029

反応方程式

hydrochloric acid

7-Cyano-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid benzyl ester

sodium hydroxide

water ethanol

→

compound

収率 85.0%

2,3,4,5-Tetrahydro-1H-1-benzazepine-7,9-di-carboxylic acid

収率 85.0%

溶媒

water

反応条件

後処理

1. 1
   温度After cooled
2. 2
   ろ過The deposited crystal was collected by filtration
3. 3
   洗浄washed with water
4. 4
   その他dried

実験手順

7-Cyano-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid benzyl ester (3.30 g) and sodium hydroxide (2 g) in a mixed solution of water-ethanol (1:1, 60 ml) was refluxed for 8 hours. After cooled, water (100 ml) was added to the reaction mixture, which was then rendered to have pH 3 with concentrated hydrochloric acid. The deposited crystal was collected by filtration, washed with water and dried to give the intended compound 1.84 g (85.0%), which was then recrystallized from ethanol to give slightly yellow crystal. M.P.: 287°-288° C.

出典