反应详情

To a cold (0° C.) solution of tert-butyl 4-[4-(acetylamino)-3-hydroxyphenyl]-2-amino-6-{2-(cyclopropylmethoxy)-6-[(4-methoxybenzyl)oxy]phenyl}nicotinate (1.00 g, 1.60 mmol) in THF (15.0 mL) under argon atmosphere was added a solution of sodium bis(2-methoxyethoxy)aluminum hydride (3.7 N in toluene, 1.25 mL, 6.39 mmol) in THF (2 mL) dropwise. After being stirred for 5 hrs., a solution of sodium bis(2-methoxyethoxy)aluminum hydride (3.7 N in toluene, 0.833 mL, 4.26 mmol) in THF (1 mL) was added to the mixture at 0° C., then the mixture was allowed to warm to room temperature, and the stirring was continued overnight. The mixture was quenched with ethyl acetate and poured into saturated aqueous sodium potassium tartarate. The extracted organic phase was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give 5-[2-amino-6-{2-(cyclopropylmethoxy)-6-[(4-methoxybenzyl)oxy]phenyl}-3-(hydroxymethyl)-4-pyridinyl]-2-(ethylamino)phenol.; LC-MS (m/z=542 M+1)

1. waitthe stirring was continued overnight
2. customThe mixture was quenched with ethyl acetate
3. additionpoured into saturated aqueous sodium potassium tartarate
4. washThe extracted organic phase was washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure