HRID1169139

反应详情

EQUATION

反应方程式

HRID 1169139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.86 g of N-(6-Chloroimidazo[1,2-b]pyridazine-2-carbonyl)glycine ethyl ester was suspended in 30 ml of ethyl acetate; 1.2 g of N-chlorosuccinimide was added, followed by thermal refluxing for 20 hours. After cooling, 30 ml of tetrahydrofuran was added; the mixture was washed with an aqueous solution of sodium thiosulfate and saline, dried over magnesium sulfate and concentrated under reduced pressure; ethyl ether was added to the residue; the crystal precipitated was collected by filtration, washed with ethyl ether and dried to yield 0.552 g of the title compound.

WORKUP

后处理

  1. customrefluxing for 20 hours
  2. temperatureAfter cooling
  3. washthe mixture was washed with an aqueous solution of sodium thiosulfate and saline
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionethyl ether was added to the residue
  7. customthe crystal precipitated
  8. filtrationwas collected by filtration
  9. washwashed with ethyl ether
  10. customdried