تفاعل #4871

ord-a830c0378624496eadb696b60415d2c3

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe mixture is stirred at room temperature for 20 hours
  2. 2
    أخرىcrystalline precipitates
  3. 3
    ترشيحare collected by filtration
  4. 4
    غسيلwashed with water
  5. 5
    workup.DISSOLUTIONThe crystals are dissolved in chloroform
  6. 6
    غسيلwashed with water
  7. 7
    أخرىdried
  8. 8
    أخرىThen, the chloroform solution is evaporated under reduced pressure
  9. 9
    أخرىto remove solvent
  10. 10
    workup.ADDITION100 ml of ethyl acetate are added to the residue
  11. 11
    أخرىto stand at room temperature
  12. 12
    أخرىCrystalline precipitates thus
  13. 13
    أخرىobtained
  14. 14
    ترشيحare collected by filtration
  15. 15
    أخرىdried

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04727071uspto-grants-1988_02