反应详情

To an ice-cold solution of 1,4-dioxane (10 mL) and MeOH (2 mL) was added 4,6-dichloro-2-ethyl-5-fluoropyrimidine (1.0 g, 5.13 mmol), N-methylpiperazine (626 uL, 5.64 mmol) and DIPEA (1.97 mL, 12.4 mmol) sequentially. The solution was then stirred at room temperature for 2 h. After the reaction was complete, anhydrous hydrazine (1.29 mL, 99 mmol) was added. The resulting suspension was heated at 90° C. in a oil bath for 2 h until the intermediate was consumed. Evaporation of the solvent gave a light yellow solid. The solid was dissolved in CH2Cl2 (100 mL) and washed with 1 N HCl. The aqueous phase was back-extracted with DCM (50 mL). The combined organic layers were dried over anhydrous Na2SO4. Evaporation of the solvent gave a light yellow residue as the desired product (890 mg, 69%).

1. temperatureThe resulting suspension was heated at 90° C. in a oil bath for 2 h until the intermediate
2. customwas consumed
3. customEvaporation of the solvent
4. customgave a light yellow solid
5. washwashed with 1 N HCl
6. extractionThe aqueous phase was back-extracted with DCM (50 mL)
7. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
8. customEvaporation of the solvent