反应详情

A solution of 2-chloromethyl-pyrimidin-4-ylamine (Imperial Chemical Industries PLC Patent: U.S. Pat. No. 4,447,441 A1, 1984; 300 mg, 2.1 mmol) in methanol (25 mL) is treated with piperidine-4-carboxylic acid tert-butylamide (404 mg, 2.19 mmol) and TEA (0.872 mL, 6.27 mmol). The resulting mixture is heated at reflux overnight. DCM (25 mL) and water (25 mL) are added followed by NaOH 1M to adjust at pH 10. The organic phase is separated. The aqueous phase is extracted with DCM (25 mL). The combined organic phases are dried over MgSO4, filtered and evaporated. Evaporation of the solvent yields the crude product (0.57 g, 94%) as a brownish solid; LC-MS A: tR=0.40 min; [M+H]+=292.14.

1. temperatureThe resulting mixture is heated
2. temperatureat reflux overnight
3. customThe organic phase is separated
4. extractionThe aqueous phase is extracted with DCM (25 mL)
5. dry with materialThe combined organic phases are dried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customEvaporation of the solvent