反応 #1478574

反応方程式

p-nitroaniline

calcium carbonate

chloroacetamide

→

pure product

収率 58.0%

2-(4-nitrophenylamino)acetamide

収率 58.0%

溶媒

water ethanol

反応条件

後処理

1. 1
   温度was refluxed for 42 hours
2. 2
   ろ過The resulting mixture was filtered while hot and
3. 3
   温度to cool
4. 4
   ろ過the crystals were filtered off by suction
5. 5
   洗浄washed with absolute ethanol
6. 6
   その他After drying
7. 7
   その他87.9 g of crude product were obtained
8. 8
   その他After two recrystallizations from acetonitrile

実験手順

A mixture of p-nitroaniline (55.2 g, 0.4 mol), calcium carbonate (80 g) and chloroacetamide (149.6 g, 1.6 mol) in 350 ml of water/ethanol (1/1) was refluxed for 42 hours. The resulting mixture was filtered while hot and allowed to cool, and the crystals were filtered off by suction, reslurried in water and then washed with absolute ethanol. After drying, 87.9 g of crude product were obtained. After two recrystallizations from acetonitrile, 45.3 g of pure product were obtained (melting point=178° C.).

出典