反应详情

To a solution of 1-(2,4-dichloro-6-morpholin-4-yl-pyrimidin-5-yloxy)-3,3-dimethyl-butan-2-ol (255 mg, 0.73 mmol) in THF (10 mL) was added sodium hydride (87 mg, 2.18 mmol, 60% dispersion in mineral oil) and the mixture was stirred at RT for 1.5 hours. The reaction was quenched with saturated aqueous ammonium chloride solution then extracted with ethyl acetate (×2). The combined organic layers were dried (Na2SO4) then passed through a pad of silica eluting with ethyl acetate. The relevant fractions were concentrated in vacuo giving 7-tert-Butyl-2-chloro-4-morpholin-4-yl-6,7-dihydro-[1,4]dioxino[2,3-d]pyrimidine as a white solid (250 mg, 100%). LCMS: RT=3.64 min, [M+H]+=314/316.

1. customThe reaction was quenched with saturated aqueous ammonium chloride solution
2. extractionthen extracted with ethyl acetate (×2)
3. dry with materialThe combined organic layers were dried (Na2SO4)
4. concentrationThe relevant fractions were concentrated in vacuo