반응 #595370

반응 방정식

4-bromo-2-fluoro-5-methylbenzoic acid

SOCl2

CH3OH

→

title compound

methyl 4-bromo-2-fluoro-5-methylbenzoate

반응 조건

후처리

1. 1
   기타The solvent was removed in vacuo
2. 2
   workup.ADDITIONthe residue was diluted with EtOAc
3. 3
   세척washed with H2O, brine
4. 4
   건조dried over anhydrous Na2SO4
5. 5
   농축concentrated
6. 6
   세척The resulting crude solid was washed with PE

실험 절차

To a solution of 4-bromo-2-fluoro-5-methylbenzoic acid (i-2a) (1.87 g, 8 mmol) in CH3OH (50 mL) at 0° C. was added SOCl2 (6 mL, 80 mmol) dropwise. Then the mixture was heated to 80° C. for 2 h. The solvent was removed in vacuo and the residue was diluted with EtOAc and washed with H2O, brine, dried over anhydrous Na2SO4, and concentrated. The resulting crude solid was washed with PE to give the title compound as a yellow solid. 1H NMR (400 MHz, CDCl3) δ 7.80 (1H, d), 7.37 (1H, d), 3.92 (3H, s), 2.39 (3H, s).

출처