반응 #71513

반응 방정식

triethylsilane

5-[3-(trifluoroacetamido)propynyl]cytidine

→

5-[3-(trifluoroacetamido)propyl]cytidine

수율 71.0%

용매

methanol

반응 조건

후처리

1. 1
   여과the reaction mixture was filtered through glass fiber
2. 2
   농축the filtrate was concentrated under reduced pressure
3. 3
   기타giving a dark brown residue
4. 4
   기타The residue was purified by flash chromatography
5. 5
   기타Removal of solvent from the appropriate fractions

실험 절차

5-[3-(trifluoroacetamido)propynyl]cytidine (1.25 g, 3.19 mmol, 1.00 equiv.) was dissolved in methanol (30 mL). Palladium hydroxide (0.25 g, 20 wt./wt. % based on propynyl cytidine) and triethylsilane (3.71 g, 31.90 mmol, 10.00 equiv.) were added to the reaction mixture. After 20-24 hours at ambient temperature, the reaction mixture was filtered through glass fiber and the filtrate was concentrated under reduced pressure giving a dark brown residue. The residue was purified by flash chromatography. Removal of solvent from the appropriate fractions afforded 0.85 g (71%) of 5-[3-(trifluoroacetamido)propyl]cytidine as a cream colored solid, which was confirmed by 1H-NM.

출처