反应详情

温度

85 °C

To a solution of 4-chloro-6-[(2R)-2,4-dimethyl-1-piperazinyl]-5-fluoro-2-methylpyrimidine (9.6 g, assumed 31.4 mmol) in 1,4-dioxane (126 mL) was added hydrazine monohydrate (8.5 mL, 175 mmol). The mixture was heated at 85° C. and stirred for 24 h. The mixture was cooled to room temperature and then concentrated in vacuo. The residue was partitioned between DCM (200 mL) and sat. aq. NaHCO3 (100 mL). The aqueous phase was extracted with a fresh portion of DCM (50 mL), and the combined organic phase was dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give crude 4-[(2R)-2,4-dimethyl-1-piperazinyl]-5-fluoro-6-hydrazino-2-methylpyrimidine (8.04 g, >100% crude yield) as a dark orange oil. LCMS: (M+H)+: 254.9.

1. temperatureThe mixture was cooled to room temperature
2. concentrationconcentrated in vacuo
3. customThe residue was partitioned between DCM (200 mL) and sat. aq. NaHCO3 (100 mL)
4. extractionThe aqueous phase was extracted with a fresh portion of DCM (50 mL)
5. dry with materialthe combined organic phase was dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo