HRID1930409

反应详情

EQUATION

反应方程式

HRID 1930409 的结构方程式

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

2-(4-Fluoro-2-methyl-5-nitrophenyl)acetic acid (18.43 g, 86.5 mmol, 1.00 eq) and cone. H2SO4 (4.00 ml) were combined in EtOH (300 ml) and stirred with heating at 85° C. After 2.5 h, the completed reaction was cooled to RT and concentrated as completely as possible. The residue was dissolved in MTBE (250 ml) and washed with H2O (2×) and brine (2×), dried (MgSO4), filtered and evaporated to afford ethyl 2-(4-fluoro-2-methyl-5-nitrophenyl)acetate (16.79 g, 81% yield) as a dark orange oil which was used as is in the next reaction. MS (ESI) m/z: 242.0 (M+H)+.

WORKUP

后处理

  1. customthe completed reaction
  2. temperaturewas cooled to RT
  3. concentrationconcentrated as completely as possible
  4. dissolutionThe residue was dissolved in MTBE (250 ml)
  5. washwashed with H2O (2×) and brine (2×)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customevaporated