Reaktion #344320

Reaktionsgleichung

hydrochloric acid

7-cyanobenzo-1,2,3-thiadiazole

diethyl ether

→

ethyl benzo-1,2,3-thiadiazole-7-carboximidate hydrochloride

Lösungsmittel

tetrahydrofuran

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITto stand for another 4 days in the refrigerator
2. 2
   FiltrationThe solid is then filtered off
3. 3
   Waschenwashed with diethyl ether
4. 4
   Sonstigedried

Vorschrift

7.2 g of 7-cyanobenzo-1,2,3-thiadiazole are dissolved at 45° C. in 60 ml of absolute ethanol and 20 ml of tetrahydrofuran, and the solution is cooled to 0° C. and saturated with gaseous hydrochloric acid in the course of 1 hour at 0° C. to 15° C., with the exclusion of moisture. The reaction mixture is then stored for 24 hours in the refrigerator, treated with 70 ml of absolute diethyl ether and allowed to stand for another 4 days in the refrigerator. The solid is then filtered off, washed with diethyl ether and dried. This gives 9.4 g of compound 5.2 in the form of beige crystals of m.p. 270°-272° C.

Quelle