反応 #595370

反応方程式

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

SOCl2

CH3OH

→

title compound

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

反応条件

後処理

1. 1
   その他The solvent was removed in vacuo
2. 2
   workup.ADDITIONthe residue was diluted with EtOAc
3. 3
   洗浄washed with H2O, brine
4. 4
   乾燥dried over anhydrous Na2SO4
5. 5
   濃縮concentrated
6. 6
   洗浄The resulting crude solid was washed with PE

実験手順

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).

出典