HRID393278

反应详情

EQUATION

反应方程式

HRID 393278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of NaNO2 (111 mg, 1.61 mmol) in water (1 mL) was added over 5 min to an ice-cold suspension of ethyl 5-(4-aminophenyl)-2-methyl-3-furanecarboxylate (395 mg, 1.61 mmol) in aqueous 1 M H2SO4 solution (12 mL). The reaction mixture was stirred at 0° C. for 20 min then was heated to 90° C. for 1 h. The cooled mixture was extracted with EtOAc. The organic layer was washed with water (2×) and brine, dried (MgSO4), filtered and concentrated under reduced pressure to yield the title compound (78 mg, 20% yield) as a white solid.

WORKUP

后处理

  1. temperaturethen was heated to 90° C. for 1 h
  2. extractionThe cooled mixture was extracted with EtOAc
  3. washThe organic layer was washed with water (2×) and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure