反应详情

To a solution of 2-Chloro-4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-benzoic acid methyl ester (i.e. the product of Step 1, 2.20 g) in CH2Cl2 was added a solution of diisobutyl aluminium hydride (1 M in CH2Cl2 , 10.7 mL) at −78° C. and kept at this temperature for 30 min. MeOH (25 mL) was added carefully and the mixture was allowed to warm to room temp, when aqueous K-Na-tartrate solution was added. The layers were separated and the aqueous phase was extracted with CH2Cl2, combined organic layers were washed with water, dried (Na2SO4) and evaporated. The residue was purified by flash chromatography on silica gel to obtain the title compound (1.35 g, 66%) and 2-Chloro-4-[5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-benzyl alcohol (0.49 g, 24%).

1. customThe layers were separated
2. extractionthe aqueous phase was extracted with CH2Cl2
3. washwere washed with water
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customThe residue was purified by flash chromatography on silica gel