반응 #4873

반응 방정식

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

수율 64.2%

용매

dimethylsulfoxide

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature for 5 hours
2. 2
   기타crystalline precipitates
3. 3
   여과are collected by filtration
4. 4
   workup.DISSOLUTIONThe crystals are dissolved in ethyl acetate
5. 5
   세척the solution is washed with water
6. 6
   기타dried
7. 7
   농축The solution is concentrated under reduced pressure
8. 8
   기타to remove solvent
9. 9
   기타Then, the residue is crystallized with isopropyl ether
10. 10
    여과collected by filtration

실험 절차

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.

출처