HRID1845158

反应详情

EQUATION

反应方程式

HRID 1845158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of methyl 4′-methyl-5-(methylsulfonyl)biphenyl-3-carboxylate (0.55 g, 1.8 mmol), MeOH (50 mL) and 2N aq. NaOH (4 mL) was stirred at 50° C. for 3 h. After cooling the mixture was concentrated in vacuo and acidified with 1N aq. HCl to pH<4 and extracted with EtOAc (100 mL). The organic layer was washed with brine, dried (Na2SO4), and concentrated to yield a white solid. LC-MS: 289.3 [M−1]−; 1H NMR (400 MHz, CDCl3): δ 8.61 (t, 1H, J=1.6 Hz), 8.59 (t, 1H, J=1.6 Hz), 8.39 (t, 1H, J=1.6 Hz), 7.58 (d, 2H, J=8.0 Hz), 7.33 (d, 2H, J=8.0 Hz), 3.15 (s, 3H), 2.44 (s, 3H).

WORKUP

后处理

  1. temperatureAfter cooling the mixture
  2. concentrationwas concentrated in vacuo
  3. extractionextracted with EtOAc (100 mL)
  4. washThe organic layer was washed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated
  7. customto yield a white solid