反应详情

To a solution of 2-cyclopropyl-2-(2,4-dichloro-6-morpholin-4-yl-pyrimidin-5-yloxy)-ethanol (215 mg, 0.64 mmol) in THF (10 mL) was added sodium hydride (71 mg, 1.93 mmol, 65% dispersion in mineral oil) and the reaction stirred for 2 hours. The reaction was quenched with saturated aqueous ammonium chloride solution (15 mL) and water (5 mL) then extracted with ethyl acetate (3×20 mL). The combined organic phases were washed with brine (15 mL), dried (Na2SO4) then concentrated in vacuo to give 2-Chloro-6-cyclopropyl-4-morpholin-4-yl-6,7-dihydro-[1,4]dioxino[2,3-d]pyrimidine as a white solid (191 mg, quantitative). LCMS: RT=3.18 min, [M+H]+=298/300.

1. customThe reaction was quenched with saturated aqueous ammonium chloride solution (15 mL) and water (5 mL)
2. extractionthen extracted with ethyl acetate (3×20 mL)
3. washThe combined organic phases were washed with brine (15 mL)
4. dry with materialdried (Na2SO4)
5. concentrationthen concentrated in vacuo