HRID129602

反应详情

EQUATION

反应方程式

HRID 129602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of (E)-methyl 2-[2-(3-aminophenoxy)phenyl]-3-methoxypropenoate (0.4 g) in glacial acetic acid (2 ml) was treated with 5.8M hydrochloric acid (1 ml), at -10° C. The stirred solution was then treated with sodium nitrite (0.1 g in 2 ml of water) still at -10° C. After 30 minutes, the resulting solution (containing the diazonium salt) was added to a stirred mixture of glacial acetic acid (0.5 ml) saturated with sulphur dioxide, containing 0.1 g of cuprous chloride (effervescence). After 30 minutes, the reaction mixture was poured into water and extracted with ether. The ether extracts were neutralized with a saturated aqueous solution of sodium bicarbonate, dried and concentrated to give (E)-methyl 2-[2-(3-chlorosulphonylphenoxy)phenyl]-3-methoxypropenoate (0.14 g) as a yellow oil.

WORKUP

后处理

  1. waitAfter 30 minutes
  2. extractionextracted with ether
  3. customdried
  4. concentrationconcentrated