反応 #4871

反応方程式

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

収率 85.7%

溶媒

dimethylsulfoxide

反応条件

後処理

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

実験手順

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.

出典