반응 #9666

반응 방정식

N-(3,5-difluorophenyl) thiourea

bromine

→

5,7-difluoro-1,3-benzothiazol-2-amine

수율 90.7%

용매

DCE

DCE

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도at reflux for 2.5 h
3. 3
   기타the precipitate formed
4. 4
   여과was collected by filtration
5. 5
   세척washed with DCE
6. 6
   여과filtered
7. 7
   기타dried in a vacuum oven

실험 절차

To a suspension of N-(3,5-difluorophenyl) thiourea (3.40 g, 18.07 mmol) in DCE (95 mL) was added a solution of bromine in DCE (5 mL) below 30° C. The mixture was heated at reflux for 2.5 h, then cooled to 10° C., and the precipitate formed was collected by filtration and washed with DCE. The solid was stirred with water (200 mL), basified by treatment with conc. ammonium hydroxide, filtered, and dried in a vacuum oven to afford 5,7-difluoro-1,3-benzothiazol-2-amine (3.05 g, 90%). ret. time 2.18; m/z 187.1 (NH+); 1H NMR (400 MHz, DMSO-d6) δ 6.92 (m, 1H), 7.00 (m, 2H), 7.92 (s, 2H).

출처