反应详情

1-(3-Chloro-propyl)-3-pyridin-3-yl-urea (I-10a: 2.1 g, 9.859 mmol) in dry DMF (10 mL) was added to a solution of sodium hydride (487 mg, 10.154 mmol) in THF (2 mL) at 0° C. The reaction temperature was maintained at room temperature for 30 minutes. The reaction was monitored by TLC (100% ethyl acetate). The reaction mixture was quenched with MeOH (5 mL) at 0° C., concentrated under reduced pressure and partitioned between ice cold water and chloroform. The organic layer was dried over Na2SO4, and concentrated under reduced pressure to afford 1.7 g (97.14% yield) of 1-pyridin-3-yl-tetrahydro-pyrimidin-2-one.

1. customThe reaction mixture was quenched with MeOH (5 mL) at 0° C.
2. concentrationconcentrated under reduced pressure
3. custompartitioned between ice cold water and chloroform
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated under reduced pressure