反应详情

A 10 mL one neck round bottom flask, fitted with argon inlet and magnetic stirrer was placed in an ice bath and charged with 400 mg(1.8 mM) of 1,1,1-trifluoro-4-(4-hydroxyphenyl)-2-butanone, 400 mg(2.4 mM) of diethyl chlorophosphate, 0.15 mL of dry pyridine and 5 mL of dichloromethane at 5° C. The mixture was stirred overnight at ambient temperature, filtered to remove pyridine HCl, extracted with 0.2N HCl, extracted with water, and dried (anhydrous MgSO4). Solvent removal under reduced pressure gave a crude yield of 600 mg of a brown oil. Preparative TLC using 1:1 ethyl acetate:hexane gave 600 mg(92%) of a clear oil nmr(CDCl3) - L 1.50(m,6H), 3.0(m,4H), 4.20(m,4H), 7.15(s,4H).

1. customwas placed in an ice bath
2. filtrationfiltered
3. customto remove pyridine HCl
4. extractionextracted with 0.2N HCl
5. extractionextracted with water
6. dry with materialdried (anhydrous MgSO4)
7. customSolvent removal under reduced pressure
8. customgave a crude yield of 600 mg of a brown oil