反应详情

6.9 g of tetrabutylammonium tribromide are added in portions at room temperature to a solution of 2.6 g of 2-(3-methoxypropoxy)-phenol in 60 ml of dichloromethane and 40 ml of methanol. The reaction mixture is concentrated by evaporation and the residue is partitioned between diethyl ether and water. The organic phases are combined, dried over magnesium sulfate and concentrated by evaporation and the residue is purified by means of FC (700 g of silica gel, dichloromethane/diethyl ether 98:2) to yield the title compound: Rf (dichloromethane/diethyl ether 97: 3)=0.50; HPLC Rt =14.3 minutes; FAB-MS (M+H)+ =262.

1. concentrationThe reaction mixture is concentrated by evaporation
2. customthe residue is partitioned between diethyl ether and water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated by evaporation
5. customthe residue is purified by means of FC (700 g of silica gel, dichloromethane/diethyl ether 98:2)