Reaktion #5887

Reaktionsgleichung

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

Lösungsmittel

chloroform

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationAfter filtering off the solid
2. 2
   Sonstigethe solution is evaporated
3. 3
   Sonstigeto get a yellow solid which
4. 4
   SonstigeThe solid separated
5. 5
   Extraktionis extracted with hexane
6. 6
   Filtrationfiltered through 150 g of neutral alumina

Vorschrift

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°.

Quelle