Cl.[NH2:2][C:3]1[N:4]=[C:5](O)[C:6]2[S:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[C:7]=2[N:8]=1.O=P(Cl)(Cl)[Cl:19].CN(C)C1C=CC=CC=1>[NH4+].[OH-]>[Cl:19][C:5]1[C:6]2[S:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[C:7]=2[N:8]=[C:3]([NH2:2])[N:4]=1A suspension of 2-amino-benzo[4,5]thieno[3,2-d]pyrimidin-4-ol hydrochloride (179 mg, 0.7 mmol), POCl3 (1.5 mL), and N,N-dimethylaniline (0.15 mL) was heated at 110° C. for 3 h. The mixture was cooled to rt and the resulting suspension was added dropwise to a 0° C. solution of aq. NH4OH (19 g/L; 30 mL). The suspension was filtered and the collected solid dried to yield 87 mg (52%) of a crude solid, which was immediately used without purification.
Wird geladen…
