反应详情

Into a 200 mL round bottomed flask are added 6-amino-1,3-benzothiazole-2-thiol (2.26 g, 12.4 mmol), diphenylcyanocarbonimidate (4.43 g, 18.6 mmol) and acetonitrile (50 mL). The reaction mixture is refluxed under nitrogen atmosphere for 16 hrs. The precipitates are collected by filtration and washed with acetonitrile (15 mL). Recrystalization of the solid from ethanol affords the intermediate of N-cyano-N′-(2-mercapto-benzothiazol-6-yl)carbamimidic acid phenyl ester as white solid (1.2 g, 30%). 1H NMR (DMSO-d6) δ 7.20-7.42 (m, 8H), 7.78 (s, 1H), 10.88 (b, 1H); ESIMS: m/z 324.8 (M−H).

1. temperatureThe reaction mixture is refluxed under nitrogen atmosphere for 16 hrs
2. filtrationThe precipitates are collected by filtration
3. washwashed with acetonitrile (15 mL)
4. customRecrystalization of the solid from ethanol