HRID1086179

反应详情

EQUATION

反应方程式

HRID 1086179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

39.3 g of 5-p-methoxybenzyloxy-2-hydroxymethyl-4-pyrone is dissolved in 600 ml of pyridine, then 52.2 g of hydroxylamine hydrochloride is added thereto, and reacted at 70°-75° C. for 2.5 hours. After the reaction, the reaction mixture is concentrated to about 100 ml and, after adding 100 ml of water thereto, added to a mixed solution of 75 ml of hydrochloric acid and 225 ml of water with ice cooling. The pH is adjusted to 2-2.5, and stirring is conducted at the same temperature for 30 minutes. The formed crystals are filtered off, washed with water and then dried to obtain 16.6 f of the title compound.

WORKUP

后处理

  1. customreacted at 70°-75° C. for 2.5 hours
  2. customAfter the reaction
  3. concentrationthe reaction mixture is concentrated to about 100 ml
  4. additionafter adding 100 ml of water
  5. additionadded to a mixed solution of 75 ml of hydrochloric acid and 225 ml of water with ice cooling
  6. filtrationThe formed crystals are filtered off
  7. washwashed with water
  8. customdried