HRID384320

反应详情

EQUATION

反应方程式

HRID 384320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(3-Amino-2-methoxy-phenyl)-furan-2-carboxylic acid 9b (2.79 g, 11.97 mmol) was dissolved in 25 mL of dichloromethane followed by dropwise addition of boron tribromide (23.9 mL, 2.0 mol/L). The reaction mixture was reacted at room temperature for 1 hour. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was concentrated under reduced pressure after 5 mL of methanol was added. The residue was diluted with 100 mL of ethyl acetate and stirred for 1 hour. Then the mixture was filtered and the filter cake was dried to obtain the title compound 5-(3-amino-2-hydroxy-phenyl)-furan-2-carboxylic acid hydrobromide 9c (1.24 g, yield 47.2%) as a yellow solid.

WORKUP

后处理

  1. customThe reaction mixture was reacted at room temperature for 1 hour
  2. concentrationThe mixture was concentrated under reduced pressure after 5 mL of methanol
  3. additionwas added
  4. additionThe residue was diluted with 100 mL of ethyl acetate
  5. filtrationThen the mixture was filtered
  6. customthe filter cake was dried