反应详情

2-Chloro-4-fluorobenzenesulfonyl chloride (1.16 g; 5.0 mmol) was added to a cold solution (ice:water temperature) of 3-chloro-5-[2-(4-cyanophenyl)-ethoxy]phenol (0.689 g; 2.5 mmol; from step (ii) above) in pyridine (8 mL). The temperature was allowed to rise (slowly) to ambient overnight. The mixture was re-cooled (ice:water temperature) and ice was added to the reaction flask. After stirring for 4 hours, the pyridine was removed in vacuo. CH2Cl2 was then added and the organic layer was washed with aqueous KHSO4 and water. Drying (MgSO4), evaporation of the solvent and purification by flash chromatography (SiO2; CH2Cl2) afforded 0.84 g (72%) of the sub-title compound.

1. customto ambient overnight
2. additionwas added to the reaction flask
3. customthe pyridine was removed in vacuo
4. additionCH2Cl2 was then added
5. washthe organic layer was washed with aqueous KHSO4 and water
6. customDrying
7. custom(MgSO4), evaporation of the solvent and purification by flash chromatography (SiO2; CH2Cl2)