반응 #551579

반응 방정식

dioxane

(Z)-2-(2-tritylaminothiazol-4-yl)-2-[(2-pyrrolidon-3-yl)oxyimino]acetic acid

dioxane

methyl L-phenylalaninate

dioxane

→

(Z)-2-(2-tritylaminothiazol-4-yl)-2-[((3S)-2-pyrrolidon-3-yl)oxyimino]acetic acid methyl L-phenylalaninate salt

용매

methanol

methanol

methanol

반응 조건

후처리

1. 1
   workup.DISSOLUTIONto dissolve
2. 2
   기타Crystalline precipitates
3. 3
   여과are collected by filtration (the filtrate
4. 4
   기타thus obtained
5. 5
   workup.STIRRINGThe mixture is stirred at room temperature for 4 hours
6. 6
   기타crystalline precipitates
7. 7
   여과are collected by filtration (the filtrate

실험 절차

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.

출처