反应详情

Dissolve (R)-2-[4-methoxy-3-(3-methoxy-propoxy)-benzyl]-3-methyl butanol (14.82 g, 50 mmol) and N,N-dimethyl formamide (0.4 g, 5.5 mmol) in methyl benzene (234 ml), add phosphorus oxybromide (15.05 g, 52.5 mmol) in droplets slowly, and control the temperature below 60° C. in that process; then, let them to react at 80° C. for 2 hours; cool down to room temperature, add water (234 ml), stir for 20 minutes, and separate the layers; extract the aqueous layer with petroleum ether for three cycles, combine the organic layers and wash twice with saturated sodium bicarbonate and saturated sodium chloride respectively; dry the organic layer with anhydrous sodium sulfate, filter, and condense the filtrate so as to obtain 17.2 g of oily matter. Add mixed solvent of ethyl acetate/normal hexane (17.2 ml/34.4 ml), control the product to crystallize at −10° C., filter, and treat the filter cake by vacuum drying at room temperature, so as to obtain 13.5 g of white solid matter; the yield is 75.1%, mp: 51-53° C., chiral purity: ≧99.9%.

1. customthe temperature below 60° C.
2. customto react at 80° C. for 2 hours
3. customseparate the layers
4. extractionextract the aqueous layer with petroleum ether for three cycles
5. washwash twice with saturated sodium bicarbonate and saturated sodium chloride respectively
6. dry with materialdry the organic layer with anhydrous sodium sulfate
7. filtrationfilter
8. customcondense the filtrate so as
9. customto obtain 17.2 g of oily matter
10. additionAdd
11. customto crystallize at −10° C.
12. filtrationfilter
13. additiontreat the filter cake by vacuum
14. customdrying at room temperature