反应详情

0.213 g DTAD was added into a solution of 5-fluoro-2-nitro-phenol, 0.105 g 4,4-difluorocyclohexanol, 0.25 g triphenylphospine in 2 ml of anhydrous methylene chloride at rt. The reaction mixture was stirred at rt overnight when TLC analysis indicated the consumption of the 5-Fluoro-2-nitro-phenol. The reaction mixture was diluted with methylene chloride (50 ml) and washed with 10% potassium carbonate solution. The aqueous layer was extracted with methylene chloride (2×25 ml) and the combined organics washed with sodium hydrogecarbonate solution (25 ml). The organic layer was passed through a phase separator and concentrated in vacuo. Purification was achieved by silica gel column chromatography (solvent: 100%→1:1 iso-hexane/EtOAc).

1. customthe consumption of the 5-Fluoro-2-nitro-phenol
2. additionThe reaction mixture was diluted with methylene chloride (50 ml)
3. washwashed with 10% potassium carbonate solution
4. extractionThe aqueous layer was extracted with methylene chloride (2×25 ml)
5. washthe combined organics washed with sodium hydrogecarbonate solution (25 ml)
6. concentrationconcentrated in vacuo
7. customPurification