反应详情

A solution of 80% NaClO2 (0.19 mol) in H2O (100 mL) is added dropwise to a solution of crude 3-fluoro-4-formyl benzoic acid benzyl ester (6, 0.19 mol) and sulfamic acid (0.19 mol) in H2O (300 mL) and CH3CN (150 mL). After stirring for 1 h, the reaction mixture is poured into 1 N HCl and extracted three times with EtOAc. The combined organic layers are washed with brine, dried over MgSO4, and evaporated in vacuo. Crystals are collected by filtration and washed with ether/hexane (1:1) to give 2-fluoroterephthalic acid 4-benzyl ester (7) as white solid.

1. extractionextracted three times with EtOAc
2. washThe combined organic layers are washed with brine
3. dry with materialdried over MgSO4
4. customevaporated in vacuo
5. filtrationCrystals are collected by filtration
6. washwashed with ether/hexane (1:1)