反应详情

1.02 g of 4-(2-methoxyphenyl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile and 736 mg of sodium methanethiolate were heated at reflux in 10 ml of dimethylformamide under a nitrogen atmosphere for 1.5 hours and then poured into a mixture of diethyl ether and water. The organic phase was separated, dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using petroleum ether/ethyl acetate (3:1) for the elution. The resulting solid was recrystallized from diethyl ether/petroleum ether to give 210 mg of 4-(2-hydroxyphenyl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile of melting point 139°-140° C.

1. customThe organic phase was separated
2. dry with materialdried over sodium sulphate
3. customevaporated
4. customThe residue was chromatographed on silica gel
5. washfor the elution
6. customThe resulting solid was recrystallized from diethyl ether/petroleum ether