反应详情

A 11.37 g (29.12 mmol) portion of ethyl 3-[1-benzyloxy-3-(isoamyloxycarbonyl)cyclobutan-3-yl]-3-oxopropionate was dissolved in 100 ml of methanol to which, while cooling in an ice bath and stirring, was subsequently added 441 mg (11.65 mmol) of sodium tetrahydroborate. After 10 minutes of stirring at the same temperature, to this was gradually added saturated ammonium chloride aqueous solution. After evaporation of methanol under a reduced pressure, ethyl acetate was added to the thus obtained residue to effect separation of layers. The resulting organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under a reduced pressure to give 11.41 g (29.07 mmol) of the title compound. The thus obtained compound was used in the following reaction without purification.

1. temperaturewhile cooling in an ice bath
2. stirringAfter 10 minutes of stirring at the same temperature
3. customAfter evaporation of methanol under a reduced pressure, ethyl acetate
4. additionwas added to the thus obtained residue
5. customseparation of layers
6. washThe resulting organic layer was washed with saturated brine
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationAfter filtration
9. customthe solvent was evaporated under a reduced pressure