反应详情

Following the method of Perez et al. (Synthesis 1983, 402), to a stirred solution of 0.27 g (0.9 mmol) (2-amino-5-cyano-6-phenyl-pyrimidin-4-ylsulfanyl)-acetic acid methyl ester in 25 ml methanol was added 0.17 ml (0.9 mmol) sodium methylate solutiuon (5.4M in methanol) and stirring continued for 16 hours at reflux. The reaction mixture was then concentrated in vacuo to ca 5 ml and the resulting crystals collected by filtration and washed with ether/methanol (10/1) to afford 0.2 g (74%) 2,5-diamino-4-phenyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester as a yellow crystalline solid. ES-MS m/e (%): 301 (M+H+, 100), 269 ([M+H-MeOH]+, 45).

1. customthe method of Perez et al. (Synthesis 1983, 402)
2. temperatureat reflux
3. concentrationThe reaction mixture was then concentrated in vacuo to ca 5 ml
4. filtrationthe resulting crystals collected by filtration
5. washwashed with ether/methanol (10/1)