反応 #1990913

反応方程式

bromine

1-(2-phenoxyphenyl)thiourea

water

sodium hydroxide

→

2-amino-4-phenoxybenzothiazole

収率 48.7%

溶媒

chloroform

chloroform

反応条件

後処理

1. 1
   温度cooling during 40 minutes
2. 2
   温度After refluxing for 1 hour and 40 minutes
3. 3
   洗浄The chloroform layer was washed with water
4. 4
   乾燥dried over magnesium sulfate
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他to give crystals, which
7. 7
   その他were recrystallized twice from isopropyl alcohol

実験手順

To a mixture of 1-(2-phenoxyphenyl)thiourea (53.4 g) in chloroform (100 ml) was added dropwise a solution of bromine (35.0 g) in chloroform (50 ml) with stirring under ice-cooling during 40 minutes. After refluxing for 1 hour and 40 minutes, the mixture was cooled to ambient temperature. To the resultant mixture was added water and then the mixture was alkalified with 5% sodium hydroxide aqueous solution. The chloroform layer was washed with water, dried over magnesium sulfate, concentrated under reduced pressure to give crystals, which were recrystallized twice from isopropyl alcohol to give 2-amino-4-phenoxybenzothiazole (25.8 g). mp: 135°-137° C.

出典