تفاعل #55541

ord-d14356388db74f24bf1b93ce184f6b67

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزAfter concentrating the resultant solution in vacuo
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  3. 3
    غسيلwashed with an aqueous solution of sodium bicarbonate
  4. 4
    تجفيفa saturated aqueous solution of sodium chloride in turn, and dried over magnesium sulfate
  5. 5
    تركيزAfter concentrating the resultant solution in vacuo

الإجراء التجريبي

A solution of ethyl 2-(2-tritylaminothiazol-4-yl)-2-allyloxyiminoacetate (syn isomer, 8.7 g), 50% formic acid (42.5 ml) and tetrahydrofuran (42.5 ml) was stirred at 60° C. for 40 minutes. After concentrating the resultant solution in vacuo, the residue was dissolved in ethyl acetate, washed with an aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride in turn, and dried over magnesium sulfate. After concentrating the resultant solution in vacuo, the residue was subjected to column chromatography on silica gel with benzene and ethyl acetate in turn, to give ethyl 2-(2-aminothiazol-4-yl)-2-allyloxyiminoacetate (syn isomer, 3.7 g), mp. 102° to 104° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04220761uspto-grants-1980_09