反应 #4871

反应方程式

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

收率 85.7%

溶剂

dimethylsulfoxide

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature for 20 hours
2. 2
   其他crystalline precipitates
3. 3
   过滤are collected by filtration
4. 4
   洗涤washed with water
5. 5
   workup.DISSOLUTIONThe crystals are dissolved in chloroform
6. 6
   洗涤washed with water
7. 7
   其他dried
8. 8
   其他Then, the chloroform solution is evaporated under reduced pressure
9. 9
   其他to remove solvent
10. 10
    workup.ADDITION100 ml of ethyl acetate are added to the residue
11. 11
    其他to stand at room temperature
12. 12
    其他Crystalline precipitates thus
13. 13
    其他obtained
14. 14
    过滤are collected by filtration
15. 15
    其他dried

实验过程

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.

来源