反应 #4873

反应方程式

water

potassium carbonate

ethyl (Z)-2-(2-tritylaminothiazol-4-yl)-2-hydroxyiminoacetate

1-methyl-3-bromo-2-pyrrolidone

→

ethyl (Z)-2-(2-tritylaminothiazol-4-yl)-2-[(1-methyl-2-pyrrolidon-3-yl)oxyimino]acetate

收率 64.2%

溶剂

dimethylsulfoxide

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature for 5 hours
2. 2
   其他crystalline precipitates
3. 3
   过滤are collected by filtration
4. 4
   workup.DISSOLUTIONThe crystals are dissolved in ethyl acetate
5. 5
   洗涤the solution is washed with water
6. 6
   其他dried
7. 7
   浓缩The solution is concentrated under reduced pressure
8. 8
   其他to remove solvent
9. 9
   其他Then, the residue is crystallized with isopropyl ether
10. 10
    过滤collected by filtration

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.

来源