[Sn](Cl)Cl.[F:4][C:5]1[CH:6]=[CH:7][C:8]2[C:12]([C:13]#[N:14])=[C:11]([NH:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[N+:22]([O-])=O)[S:10][C:9]=2[CH:25]=1.O>Cl.C(O)C>[NH2:14][C:13]1[C:12]2[C:8]3[CH:7]=[CH:6][C:5]([F:4])=[CH:25][C:9]=3[S:10][C:11]=2[NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[N:22]=1Tin(II) chloride (50 g) was dissolved in a 18% hydrochloric acid (250 ml) solution heated to 50° C., and a suspension of 6-fluoro-2-(2-nitroanilino)benzo[b]thiophene-3-carbonitrile (20 g) in ethanol (280 ml) was added. The mixture was refluxed under heating for 4 hours. Then, the reaction mixture was cooled to 40° C. and poured into water (1 L) and the mixture was stood still for 30 minutes. The precipitated crystals were filtered by suction and washed with water (500 ml) to give 12-amino-3-fluoro-6H-[1]benzothieno[2,3-b][1,5]benzodiazepine.1 hydrochloride (15 g).
Loading…
