反应详情

To a solution of 1-cyclopropyl-2-(2,4-dichloro-6-morpholin-4-yl-pyrimidin-5-yloxy)-ethanol (196 mg, 0.59 mmol) in THF (10 mL) was added sodium hydride (65 mg, 1.77 mmol, 65% dispersion in mineral oil) and the reaction mixture stirred at RT for 4 hours. The reaction was quenched with saturated aqueous ammonium chloride solution (15 mL) then extracted with ethyl acetate (3×20 mL). The combined organic phases were dried (Na2SO4) and concentrated in vacuo giving 2-Chloro-7-cyclopropyl-4-morpholin-4-yl-6,7-dihydro-[1,4]dioxino[2,3-d]pyrimidine as a white solid (205 mg, quantitative). LCMS: RT=3.19 min, [M+H]+=298/300.

1. customThe reaction was quenched with saturated aqueous ammonium chloride solution (15 mL)
2. extractionthen extracted with ethyl acetate (3×20 mL)
3. dry with materialThe combined organic phases were dried (Na2SO4)
4. concentrationconcentrated in vacuo