HRID580299

反应详情

EQUATION

反应方程式

HRID 580299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 6-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)-furo[2,3-b]-pyridine-5-carboxylic acid (11.7 g, 0.039 mol) in 100 mL dimethoxyethane (DME) is added 7.3 mL acetic anhydride and 3.9 mL pyridine. After stirring 24 hours at room temperature, the solids are filtered and washed with ether and the mother liquor is concentrated by adding xylene to aid removal of pyridine. The residue is triturated with ether to obtain solids which are combined with the first crop to give 11.1 g (100%) of product. Recrystallization from 2:1 ethyl acetatehexane gives an analytical sample mp 193°-205° C.

WORKUP

后处理

  1. filtrationthe solids are filtered
  2. washwashed with ether
  3. concentrationthe mother liquor is concentrated
  4. additionby adding xylene
  5. customremoval of pyridine
  6. customThe residue is triturated with ether
  7. customto obtain solids which