反应详情

温度

20 °C

Add 191 g of 2-chloro-2',4'-difluoroacetophenone (Aldrich Chemical Co.) to a mixture of 246 g of sodium acetate, 3 g of Nal, and 3 L of DMF. Stir the mixture at 20° C. for 18 hr. then concentrate it to 1 L. Pour the residue into 6 L of cold dilute aqueous HCl and extract with EtOAc. Wash the extract with brine, dry it over anhydrous Na2SO4, filter the so-formed mixture, and evaporate the filtrate to leave a residue. Chromatograph the residue on silica gel, eluting with CH2Cl-2-hexane to obtain 198 g of the title compound. ##STR101##

1. concentrationthen concentrate it to 1 L
2. additionPour the residue into 6 L of cold dilute aqueous HCl
3. extractionextract with EtOAc
4. washWash the
5. extractionextract with brine
6. dry with materialdry it over anhydrous Na2SO4
7. filtrationfilter the so-formed mixture
8. customevaporate the filtrate
9. customto leave a residue
10. washChromatograph the residue on silica gel, eluting with CH2Cl-2-hexane