HRID129601

反应详情

EQUATION

反应方程式

HRID 129601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phosphoryl chloride (7.8 ml) was added dropwise to a stirred solution of (E)-methyl 2-[2-(3-formamidophenoxy)phenyl]-3-methoxypropenoate (13.67 g) in methanol (100 ml), the temperature during the addition being kept below 50° C. with the aid of a cooling bath. After stirring for 20 minutes, the reaction mixture was poured into water (500 ml), neutralized with sodium bicarbonate and extracted with ether. The extracts were dried and concentrated to give a yellow oil which was chromatographed using ether as the eluant to give (E)-methyl 2-[2-(3-aminophenoxy)phenyl]-3-methoxypropenoate (8.57 g, 68% yield) as a yellow solid, m.p. 83°-85° C.

WORKUP

后处理

  1. additionthe temperature during the addition
  2. custombeing kept below 50° C. with the aid of a cooling bath
  3. extractionextracted with ether
  4. customThe extracts were dried
  5. concentrationconcentrated
  6. customto give a yellow oil which
  7. customwas chromatographed