反应详情

To a suspension of NaOH (2.8 g, 70.02 mmol) in THF (10 ml) added 4-chloro phenol (1 g, 7.78 mmol) and stirred for 15 min at r.t. Reaction mixture was cooled to 0° C. Cyclohexanone (7.62 g, 77.8 mmol) was added, followed by drop wise addition of anhydrous CHCl3 (2.5 ml, 31.12 mmol) over a period of 15-20 min. The reaction mixture was stirred for 14-18 hr allowing the temperature to rise to room temperature. Reaction mixture was neutralized with (HCl, pH˜7) and was extracted with EtOAc (3×50 mL). The organic phase were successively washed with 2% HCl (50 mL), brine (50 mL) and dried over Na2SO4. After evaporation of solvent, the residue was used as such for the next step.

1. customReaction mixture
2. temperaturewas cooled to 0° C
3. stirringThe reaction mixture was stirred for 14-18 hr
4. customto rise to room temperature
5. customReaction mixture
6. extractionwas extracted with EtOAc (3×50 mL)
7. washThe organic phase were successively washed with 2% HCl (50 mL), brine (50 mL)
8. dry with materialdried over Na2SO4
9. customAfter evaporation of solvent