反应 #674375

反应方程式

4-iodo-2-bromobenzoic acid

H2SO4

EtOH

→

compound

收率 92.0%

Ethyl 2-bromo-4-iodobenzoate

收率 92.0%

反应条件

后处理

1. 1
   温度The reaction mixture was cooled to 25° C.
2. 2
   浓缩concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was diluted with EtOAc (2×100 mL)
4. 4
   洗涤washed with water (100 mL)
5. 5
   洗涤The combined EtOAc extracts were washed with brine
6. 6
   干燥dried over Na2SO4
7. 7
   浓缩concentrated under reduced pressure

实验过程

To a stirred solution of 4-iodo-2-bromobenzoic acid (5 g, 15.29 mmol) in EtOH (100 mL) was added H2SO4 (5 mL), and the reaction mixture was heated at 80° C. for 18 h. The reaction mixture was cooled to 25° C. and concentrated under reduced pressure. The residue was diluted with EtOAc (2×100 mL) and washed with water (100 mL). The combined EtOAc extracts were washed with brine, dried over Na2SO4 and concentrated under reduced pressure to afford the compound as a pale yellow solid (5 g, 92%): 1H NMR (400 MHz, DMSO-d6) δ 8.04 (d, J=1.2 Hz, 1H), 7.71 (d, J=7.6 Hz, 1H), 7.51 (d, J=8.4 Hz, 1H), 4.41 (q, J=7.2 Hz, 2H), 1.41 (t, J=7.2 Hz, 3H).

来源