Reacción #551579

ord-e73121a1c5124337a6374f6f626d0f7e

Condiciones de reacción

Temperatura
50°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.DISSOLUTIONto dissolve
  2. 2
    OtroCrystalline precipitates
  3. 3
    Filtraciónare collected by filtration (the filtrate
  4. 4
    Otrothus obtained
  5. 5
    workup.STIRRINGThe mixture is stirred at room temperature for 4 hours
  6. 6
    Otrocrystalline precipitates
  7. 7
    Filtraciónare collected by filtration (the filtrate

Procedimiento

30 g of (Z)-2-(2-tritylaminothiazol-4-yl)-2-[(2-pyrrolidon-3-yl)oxyimino]acetic acid and 60 ml of methanol are added to 100 ml of dioxane containing 0.5 g of methyl L-phenylalaninate, and the mixture is heated at 50° C. to dissolve said acid therein. 700 ml of dioxane are added to the solution, and the mixture is stirred at room temperature for 5 hours. Crystalline precipitates are collected by filtration (the filtrate is hereinafter referred to as "Filtrate I"), and 14.3 g of the crude product thus obtained are dissolved in 24 ml of methanol. 280 ml of dioxane are added to the methanol solution. The mixture is stirred at room temperature for 4 hours, and crystalline precipitates are collected by filtration (the filtrate is hereinafter referred to as "Filtrate II"). 12.2 g of (Z)-2-(2-tritylaminothiazol-4-yl)-2-[((3S)-2-pyrrolidon-3-yl)oxyimino]acetic acid methyl L-phenylalaninate salt are obtained.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04547494uspto-grants-1985_10