反应详情

To a solution of 13.7 g of 3-hydroxybenzamide and 25.6 of benzyl bromide in acetone (400 ml) were added 25.6 g of potassium carbonate at RT. The mixture was then refluxed for 6 h after which time the reaction was completed according to TLC analysis (CH2Cl2/MeOH: 20/1). The reaction mixture was cooled to RT and partitioned between EtOAc and water, the organic layer was separated, dried over sodium sulphate and concentrated in vacuo. The crystalline residue obtained was suspended in n-hexane (200 ml), the crystals were filtered off under suction and dried in a vacuum to give 3-benzyloxy-benzamide as a white crystalline solid, mp 136°-140° C.

1. temperatureThe mixture was then refluxed for 6 h after which time the reaction
2. custompartitioned between EtOAc and water
3. customthe organic layer was separated
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated in vacuo
6. customThe crystalline residue obtained
7. filtrationthe crystals were filtered off under suction
8. customdried in a vacuum