HRID1900752

反应详情

EQUATION

反应方程式

HRID 1900752 的结构方程式

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 2-bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one (4.802 g) and thiazoline (5.815 g) was stirred at 150° C. in the stream of argon gas for 4 hours. The solvent was distilled off under reduced pressure. Chloroform was added to the residue, and extracted with 1N-HCl. After the extract was washed with chloroform, 1N-NaOH was added to bring the pH basic. Extraction was performed with chloroform, followed by washing with water. After dried, the residue was crystallized from methanol to obtain 1.885 g of a free base of the title compound as pale yellow powder (mp.: 196°-199° C.).

WORKUP

后处理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionChloroform was added to the residue
  3. extractionextracted with 1N-HCl
  4. washAfter the extract was washed with chloroform, 1N-NaOH
  5. additionwas added
  6. extractionExtraction
  7. washby washing with water
  8. customAfter dried
  9. customthe residue was crystallized from methanol