反应详情

To 2-fluoro-4-nitrobenzoic acid suspended in CH2Cl2 under Ar was added DMF then oxalyl chloride. The reaction was stirred at room temperature 1.5 h then the solvent was evaporated. The residue was dissolved in THF and ammonia gas was bubbled through the reaction for 15 min. The solvent was evaporated and the residue partitioned between EtOAc and water. The aqueous layer was extracted with EtOAc. The extracts were dried (MgSO4), filtered, and evaporated. Column chromatography (SiO2, 0-100% EtOAc/Hex) gave pure 2-fluoro-4-nitrobenzamide (E335).

1. customthe solvent was evaporated
2. dissolutionThe residue was dissolved in THF
3. customammonia gas was bubbled through the reaction for 15 min
4. customThe solvent was evaporated
5. customthe residue partitioned between EtOAc and water
6. extractionThe aqueous layer was extracted with EtOAc
7. dry with materialThe extracts were dried (MgSO4)
8. filtrationfiltered
9. customevaporated