反応 #5883

反応方程式

thiophosgene

6-amino-2-tert-butyl-5-(4-methylpiperidin-1-yl)benzothiazole

potassium bicarbonate

→

2-tert-butyl-6-isothiocyanato-5-(4-methylpiperidin-1-yl)benzothiazole

溶媒

chloroform

chloroform

chloroform

反応条件

後処理

1. 1
   温度maintaining the temperature at 0°-2°
2. 2
   ろ過The solid is filtered
3. 3
   その他the filtrate is evaporated
4. 4
   その他The solid thus obtained
5. 5
   ろ過filtered through a silica gel column
6. 6
   その他The filtrate is evaporated

実験手順

To a cooled mixture of 2.1 g of 6-amino-2-tert-butyl-5-(4-methylpiperidin-1-yl)benzothiazole and 2.8 g of potassium bicarbonate in 20 ml of chloroform is added dropwise 1.6 g of thiophosgene in 5 ml of chloroform under stirring. The stirring is continued for 2 hours maintaining the temperature at 0°-2° . The solid is filtered and the filtrate is evaporated. The solid thus obtained is dissolved in chloroform and filtered through a silica gel column. The filtrate is evaporated to give 2-tert-butyl-6-isothiocyanato-5-(4-methylpiperidin-1-yl)benzothiazole, melting at 54°-58°.

出典