反应详情

To a suspension of LiAlH4 (21 g, 558.56 mmol) in anhydrous THF (500 mL) was added a solution of 1,4-dioxa-10-aza-dispiro[4.2.4.2]tetradecan-9-one (59 g, 279.28 mmol) in anhydrous THF (400 mL) dropwise at 0° C. for 1 h. The reaction mixture was stirred at reflux for another 2 h, then quenched with water at 0° C. until no bubble escaped and filtered. The filter cake was washed with a mixture of DCM and MeOH (1/1 (v/v), 500 mL). The filtrate was concentrated in vacuo and the residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/10) to give the product as a yellow solid (52 g, 94%).

1. temperatureat reflux for another 2 h
2. customquenched with water at 0° C. until no bubble
3. filtrationfiltered
4. washThe filter cake was washed with a mixture of DCM and MeOH (1/1 (v/v), 500 mL)
5. concentrationThe filtrate was concentrated in vacuo
6. customthe residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/10)