反应详情

DIAD (280 μL, 1.42 mmol) was added at −20° C. under nitrogen atmosphere to a solution of the alcohol (143) (367 mg, 0.90 mmol), 4-hydroxy-2-(3-isopropylpyrazol-1-yl)-7-methoxy-8-methylquinazoline (141) (270 mg, 0.90 mmol) and triphenyl-phosphine (288 mg, 1.42 mmol) in dry DMF (35 mL). After 2 h, the solution was warmed up to room temperature. After 12 h, the reaction mixture was partitioned between ice-cold water and ether, organic layer was dried (Na2SO4) and evaporated. The residue was purified by column chromatography (gradient AcOEt/CH2Cl2, 1:9 to 10:0) to give the title compound (230 mg, 34%), m/z=687 (M+H)+.

1. waitAfter 12 h
2. customthe reaction mixture was partitioned between ice-cold water and ether, organic layer
3. dry with materialwas dried (Na2SO4)
4. customevaporated
5. customThe residue was purified by column chromatography (gradient AcOEt/CH2Cl2, 1:9 to 10:0)