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. in 1 h. The reaction mixture was heated to reflux and stirred for 2 h, then quenched with water at 0° C. until no bubble escaped and filtered. The filtere cake was washed with a mixture of DCM and MeOH (1/1 (v/v), 500 mL). The filterate 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. temperatureThe reaction mixture was heated
2. temperatureto reflux
3. customquenched with water at 0° C. until no bubble
4. filtrationfiltered
5. washThe filtere cake was washed with a mixture of DCM and MeOH (1/1 (v/v), 500 mL)
6. concentrationThe filterate was concentrated in vacuo
7. customthe residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/10)