反应详情

A mixture of 23.9 mL (234.1 mmol) of thiophenol, 11.1 g (58.5 mmol) of tin (II) chloride and 24.5 mL (175.6 mmol) triethylamine in acetonitrile (300 mL) was stirred for 5 min at room temperature. 10-Azido-10-methyl-2-pyrimidin-4-yl-7,8,9,10-tetrahydro-6H-pyrimido[1,2-a]azepin-4-one residue diluted in 90 mL of acetonitrile was added to this solution and the mixture was stirred for 1 h. A solution of sodium hydroxide (1M) was added and the mixture extracted with dichloromethane. After an acid-basic work-up, the residue was chromatographed on silica gel eluting with a mixture of dichloromethane/methanol in the proportions 95/5 to afford 6.3 g (58%) of a yellow solid.

1. additionwas added to this solution
2. stirringthe mixture was stirred for 1 h
3. extractionthe mixture extracted with dichloromethane
4. customAfter an acid-basic work-up, the residue was chromatographed on silica gel eluting with a mixture of dichloromethane/methanol in the proportions 95/5