反应详情

2.23 g of fresh 2-methyl-6-trifluoromethylnicotinoyl chloride are added to a mixture of 2.14 g of methyl 2-hydroxy-1-methoxy-5-methyl-4-oxocyclohex-2-enecarboxylate and 2.02 g of triethylamine in 30 ml of acetonitrile. After approximately 30 minutes, 0.065 g of potassium cyanide is added and the mixture is stirred for 18 hours. At pH 2, the mixture is subsequently partitioned between water and ethyl acetate, dried over magnesium sulfate and evaporated. Filtration on silica gel (mobile phase ethyl acetate/methanoltriethylamine 85:10:5) gives the pure methyl 2-hydroxy-1-methoxy-methyl-3-(2-methyl-6-trifluoromethylpyridine-3-carbonyl)-4-oxocyclohex-2-enecarboxylate as a viscous oil.

1. customAt pH 2, the mixture is subsequently partitioned between water and ethyl acetate
2. dry with materialdried over magnesium sulfate
3. customevaporated
4. filtrationFiltration on silica gel (mobile phase ethyl acetate/methanoltriethylamine 85:10:5)