反应详情

To a stirred and ice-cooled solution of NaOMe (904 mg, 4.68 mmol) was added 2-fluoro-5-(trifluoromethyl)benzaldehyde (500 mg, 2.60 mmol) portionwise. The dropping funnel employed was washed with THF. The resultant suspension was stirred at room temperature for 5 hr. The reaction mixture was neutralizing for acetic acid (0.3ml, 5.0 mmol), the solvent was removed. To the solid residue was added water and the mixture was extracted with CH2Cl2. The combined CH2Cl2 extracts were washed with sat. NaHCO3 aq., dried with MgSO4, and concentrated to give crude Compound 4 as a white solid. This was purified with preparative TLC to give pure Compound 4 as a white crystalline (363 mg, 68.4%).

1. washThe dropping funnel employed was washed with THF
2. stirringThe resultant suspension was stirred at room temperature for 5 hr
3. customthe solvent was removed
4. additionTo the solid residue was added water
5. extractionthe mixture was extracted with CH2Cl2
6. washThe combined CH2Cl2 extracts were washed with sat. NaHCO3 aq.
7. dry with materialdried with MgSO4
8. concentrationconcentrated
9. customto give crude Compound 4 as a white solid
10. customThis was purified with preparative TLC