HRID745355

反应详情

EQUATION

反应方程式

HRID 745355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.7 g of ethyl (Z)-2-(2-tritylaminothiazol-4-yl)-2-hydroxyiminoacetate are dissolved in 12 ml of dimethylsulfoxide, and 1.0 g of anhydrous potassium carbonate is added thereto under nitrogen gas atmosphere. The mixture is stirred at room temperature for 10 minutes. 1.2 g of 1-methyl-3-bromo-2-pyrrolidone are added to the mixture, and the mixture is stirred at room temperature for 5 hours. The reaction mixture is poured into 100 ml of water, and crystalline precipitates are collected by filtration. The crystals are dissolved in ethyl acetate, and the solution is washed with water and then dried. The solution is concentrated under reduced pressure to remove solvent. Then, the residue is crystallized with isopropyl ether and collected by filtration. 2.1 g of ethyl (Z)-2-(2-tritylaminothiazol-4-yl)-2-[(1-methyl-2-pyrrolidon-3-yl)oxyimino]acetate are obtained.

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature for 5 hours
  2. customcrystalline precipitates
  3. filtrationare collected by filtration
  4. dissolutionThe crystals are dissolved in ethyl acetate
  5. washthe solution is washed with water
  6. customdried
  7. concentrationThe solution is concentrated under reduced pressure
  8. customto remove solvent
  9. customThen, the residue is crystallized with isopropyl ether
  10. filtrationcollected by filtration