反应详情

To a solution of ethyl 4-({5-fluoro-4-[(2-{[(1 methylethyl)amino]carbonyl}phenyl)amino]-2-pyrimidinyl}amino)benzoate (1.47 g, 3.36 mmol) in THF (80 mL) was slowly added a solution of LiAlH4 (1.0M solution, 3.0 eq) at 0° C. After the addition was complete, the reaction mixture was slowly warmed up to room temperature and stirred for 16 h. The reaction mixture was quenched with 15 mL of 1.0 M Rochelle's solution. The water phase was extracted by EtOAc (2×30 mL) and the combined organic phases were washed by brine (3×30 mL) then dried over Na2SO4. The solvent was evaporated to produce a solid, which was washed with hexane (3×30 mL), then dried in vacuo to give the desired product. (1.15, 87% yield). MS: M(C21H22FN5O2)=395.44, (M+H)+=396

1. additionAfter the addition
2. customThe reaction mixture was quenched with 15 mL of 1.0 M Rochelle's solution
3. extractionThe water phase was extracted by EtOAc (2×30 mL)
4. washthe combined organic phases were washed by brine (3×30 mL)
5. dry with materialthen dried over Na2SO4
6. customThe solvent was evaporated
7. customto produce a solid, which
8. washwas washed with hexane (3×30 mL)
9. customdried in vacuo