反应详情

A suspension of 0.234 g (1.00 mmol) of the 6-bromo-2-methyl-5-nitro-3H-pyrimidin-4-one, 0.205 g (1.00 mmol) of the 2-methyl-5,6,7,8-tetrahydro-4H-thiazolo[4,5-d]azepine hydrochloride and 0.304 g (2.20 mmol) of potassium carbonate in 2.0 ml of N,N-dimethylformamide was stirred at room temperature for 60 hours. The reaction mixture was then poured into 50 ml of an ice/water mixture and the crystals formed collected by filtration. Thus, a first crop of the 2-methyl-6-(2-methyl-4,5,7,8-tetrahydro-thiazolo[4,5-d]azepin-6-yl)-5-nitro-3H-pyrimidin-4-one was obtained. The mother liquor was then evaporated and the residue chromatographed on silica gel using a 9:1 v/v mixture of dichloromethane and methanol as eluent giving a second crop of the 2-methyl-6-(2-methyl-4,5,7,8-tetrahydro-thiazolo[4,5-d]azepin-6-yl)-5-nitro-3H-pyrimidin-4-one, in total 0.252 g (0.785 mmol, yield 78.5%) as light yellow solid; m.p. >200° C.; MS: [M+H]+=322.

1. customthe crystals formed
2. filtrationcollected by filtration