反应详情

温度

50 °C

To a solution of 5-bromo-2-hydroxy-4-(4-morpholinylmethyl)benzoic acid (may be prepared as described in Description 5; 720 mg, 2.28 mmol) in N,N-dimethylformamide (10 ml) was added potassium carbonate (1102 mg, 7.97 mmol) and 4-fluorobenzyl bromide (0.62 ml, 5.01 mmol). The mixture was heated at 50° C. for 2 hours, cooled and the solvent removed in vacuo. The residue was partitioned between water (10 ml) and ethyl acetate (15 ml). The organic layer was separated, washed further with water (2×5 ml), dried (MgSO4) and the solvent removed in vacuo to give a residue. Purification by column (SiO2, 6:1-1:1 cyclohexane/ethyl acetate) gave the product as a pale yellow oil. 544 mg.

1. temperaturecooled
2. customthe solvent removed in vacuo
3. customThe residue was partitioned between water (10 ml) and ethyl acetate (15 ml)
4. customThe organic layer was separated
5. washwashed further with water (2×5 ml)
6. dry with materialdried (MgSO4)
7. customthe solvent removed in vacuo
8. customto give a residue
9. customPurification by column (SiO2, 6:1-1:1 cyclohexane/ethyl acetate)