HRID730268

反应详情

EQUATION

反应方程式

HRID 730268 的结构方程式

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Ethyl 5-nitrobenzo[d]furan-2-carboxylate. To a 250 mL round-bottomed flask was added methyl 2-(2-formyl-4-nitrophenoxy)acetate, Example 38(a), (5.3 g, 22 mmol), EtOH (110 mL) and 1,8-diazabicyclo[5.4.0]undec-7-ene (3.7 g, 24 mmol, Aldrich). The reaction mixture was magnetically stirred at 25° C. for 20 h, then concentrated to approximately half of its volume in vacuo. After cooling the mixture in an ice bath for 20 min, a precipitate formed which was collected by filtration and washed with ice cold EtOH. The resulting pale yellow solid was dried in vacuo to provide the title product. MS (ESI, pos. ion) m/z: 253 (M+H2O).

WORKUP

后处理

  1. concentrationconcentrated to approximately half of its volume in vacuo
  2. temperatureAfter cooling the mixture in an ice bath for 20 min
  3. customa precipitate formed which
  4. filtrationwas collected by filtration
  5. washwashed with ice cold EtOH
  6. customThe resulting pale yellow solid was dried in vacuo