反应详情

54.5 g of NaBH4 were added, in portions, to a solution of 150 g of (I) in 1.5 l of methanol. The mixture was refluxed for 1 hour and then concentrated, 1 l of 2N HCl was added, and the mixture was refluxed for a further hour and then extracted with CH2Cl2. The organic phase was washed with water, dried over Na2SO4 and concentrated. Distillation of the residue gave 93 g of (II) of boiling point 156°-160° C./0.2 mbar.

1. temperatureThe mixture was refluxed for 1 hour
2. concentrationconcentrated
3. addition1 l of 2N HCl was added
4. temperaturethe mixture was refluxed for a further hour
5. extractionextracted with CH2Cl2
6. washThe organic phase was washed with water
7. dry with materialdried over Na2SO4
8. concentrationconcentrated
9. distillationDistillation of the residue