反应详情

To a stirred suspension of 3,3-dimethyl-6-morpholino-1H-pyrrolo[3,2-b]pyridin-2(3H)-one (425 mg, 1.719 mmol) in toluene (14 mL) at 0° C. was added sodium bis(2-methoxyethoxy)aluminum hydride (3.3 M solution in toluene, 1.56 mL, 5.16 mmol). The reaction was stirred while warming to rt for 4 h. After this time the reaction was carefully quenched with water (5 mL) and then diluted with DCM (50 mL) and treated with saturated aqueous solution Na2S2O3 (20 mL). The separated aqueous layer was then extracted with DCM (20 mL) and the combined organic layers were washed with brine (20 mL) and then dried over MgSO4, filtered and evaporated in vacuo to give 4-(3,3-dimethyl-2,3-dihydro-1H-pyrrolo[3,2-b]pyridin-6-yl)morpholine. Mass Spectrum (ESI) m/e=234.2 (M+1).

1. customAfter this time the reaction was carefully quenched with water (5 mL)
2. additiondiluted with DCM (50 mL)
3. additiontreated with saturated aqueous solution Na2S2O3 (20 mL)
4. extractionThe separated aqueous layer was then extracted with DCM (20 mL)
5. washthe combined organic layers were washed with brine (20 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated in vacuo