反应详情

A solution of 4.16 g of the product of Step A in 4 ml of methylene chloride was admixed with 45 ml of acetic acid containing 10% of water and 0.53 g of zinc powder and the mixture was stirred for 30 minutes at room temperature. then another 0.53 g of zinc powder were added 4 times until The reaction was complete and after 3 hours contact, the mixture was filtered. The filtrate was extracted with methylene chloride and the organic phase was washed with water, dried and evaporated to dryness by azeotropic distillation with toluene to obtain 3.05 g of (R)α-methyl-3-phenoxy-benzyl (1R,cis) 2,2-dimethyl-3-[3-oxo-3-hydroxy-1-propynyl]-cyclo-propane-carboxylate.

1. waitwas complete and after 3 hours
2. filtrationcontact, the mixture was filtered
3. extractionThe filtrate was extracted with methylene chloride
4. washthe organic phase was washed with water
5. customdried
6. customevaporated to dryness by azeotropic distillation with toluene