تفاعل #4873

معادلة التفاعل

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

المردود 64.2%

المذيبات

dimethylsulfoxide

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture is stirred at room temperature for 5 hours
2. 2
   أخرىcrystalline precipitates
3. 3
   ترشيحare collected by filtration
4. 4
   workup.DISSOLUTIONThe crystals are dissolved in ethyl acetate
5. 5
   غسيلthe solution is washed with water
6. 6
   أخرىdried
7. 7
   تركيزThe solution is concentrated under reduced pressure
8. 8
   أخرىto remove solvent
9. 9
   أخرىThen, the residue is crystallized with isopropyl ether
10. 10
    ترشيحcollected by filtration

الإجراء التجريبي

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.

المصدر