反応 #5887

反応方程式

sodium hydroxide

6-Amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole

sodium bicarbonate

thiophosgene

→

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

溶媒

chloroform

water

反応条件

後処理

1. 1
   ろ過After filtering off the solid
2. 2
   その他the solution is evaporated
3. 3
   その他to get a yellow solid which
4. 4
   その他The solid separated
5. 5
   抽出is extracted with hexane
6. 6
   ろ過filtered through 150 g of neutral alumina

実験手順

To a stirred mixture of 75 g of 6-Amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole and 29 g of sodium bicarbonate in 1100 ml of chloroform at 0° is added 41 g of thiophosgene and the mixture stirred at 10° for 4 hours. After filtering off the solid, the solution is evaporated to get a yellow solid which is dissolved in water and the pH of the solution is brought to 7 by the addition of dilute sodium hydroxide. The solid separated is extracted with hexane and filtered through 150 g of neutral alumina to give 2-tert-butyl-6-isothiocyanato-5-(4-methyl-piperazin-1-yl)benzothiazole, melting at 124°-126°.

出典