반응 #4871

반응 방정식

water

potassium carbonate

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

3-bromo-2-pyrrolidone

→

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

수율 85.7%

용매

dimethylsulfoxide

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature for 20 hours
2. 2
   기타crystalline precipitates
3. 3
   여과are collected by filtration
4. 4
   세척washed with water
5. 5
   workup.DISSOLUTIONThe crystals are dissolved in chloroform
6. 6
   세척washed with water
7. 7
   기타dried
8. 8
   기타Then, the chloroform solution is evaporated under reduced pressure
9. 9
   기타to remove solvent
10. 10
    workup.ADDITION100 ml of ethyl acetate are added to the residue
11. 11
    기타to stand at room temperature
12. 12
    기타Crystalline precipitates thus
13. 13
    기타obtained
14. 14
    여과are collected by filtration
15. 15
    기타dried

실험 절차

15.8 g of ethyl (Z)-2-(2-tritylaminothiazol-4-yl)-2-hydroxyiminoacetate are dissolved in 70 ml of dimethylsulfoxide, and 5.8 g of anhydrous potassium carbonate are added thereto. The mixture is stirred at room temperature for 20 minutes. 6.6 g of 3-bromo-2-pyrrolidone are added to said mixture, and the mixture is stirred at room temperature for 20 hours. The mixture is poured into 800 ml of water, and crystalline precipitates are collected by filtration and washed with water. The crystals are dissolved in chloroform, washed with water and then dried. Then, the chloroform solution is evaporated under reduced pressure to remove solvent. 100 ml of ethyl acetate are added to the residue, and allowed to stand at room temperature. Crystalline precipitates thus obtained are collected by filtration and dried. 16.0 g of ethyl (Z)-2-(2-tritylaminothiazol-4-yl)-2-[(2-pyrrolidon-3-yl)oxyimino]acetate are obtained.

출처