反应详情

4-Amino-6-chloro-2-mercaptopyrimidine mesylate (0.30 g, 1.16 mmol) is dissolved in 3.25N sodium hydroxide (2 ml) and ethanol (1 ml) at ambient temperature followed by the addition of methyl 4-bromocrotonate (0.16 ml, 1.40 mmol). The reaction is stirred for 2 to 15 hours, quenched with excess water, extracted with methylene chloride (2×25 ml). The extracts are combined, washed with saline (25 ml), dried over sodium sulfate, concentrated in vacuo and recrystallized from hexane/ethyl acetate to give Cpd #193. mp 146-149° C.

1. customquenched with excess water
2. extractionextracted with methylene chloride (2×25 ml)
3. washwashed with saline (25 ml)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customrecrystallized from hexane/ethyl acetate
7. customto give Cpd #193