반응 #657272

반응 방정식

N-hydroxysuccinimide

dicyclohexylcarbodiimide

(Pyrimidin-2-ylsulfanyl)-acetic acid

→

(Pyrimidin-2-ylsulfanyl)-acetic acid-(2,5-dioxo-pyrrolidine-1-yl)-ester

용매

DMF

반응 조건

후처리

1. 1
   여과The residue was filtered
2. 2
   기타the filtrate was evaporated in vacuo to dryness
3. 3
   workup.DISSOLUTIONThe remaining product was dissolved
4. 4
   온도under reflux in 400 ml ethyl acetate
5. 5
   여과the hot solution was filtered
6. 6
   기타the mixture was subjected to a chromatographic purification (Florisil)
7. 7
   기타The compound was then recrystallised from ethyl acetate

실험 절차

12.31 g (107 mMol) N-hydroxysuccinimide and 22.70 g (110 mMol) dicyclohexylcarbodiimide were added at −35° C. to a solution of 18.27 g (107 mMol) (Pyrimidin-2-ylsulfanyl)-acetic acid (a) dissolved in 200 ml DMF. The reaction mixture was stirred for 16 h under argon. The residue was filtered and the filtrate was evaporated in vacuo to dryness. The remaining product was dissolved under reflux in 400 ml ethyl acetate, the hot solution was filtered and the mixture was subjected to a chromatographic purification (Florisil) using ethyl acetate. The compound was then recrystallised from ethyl acetate.

출처