반응 #41628

반응 방정식

tin(II) chloride dihydrate

4-methanesulfonyl-phenol

cesium carbonate

trans-1-acetyl-2-(5-nitro-2-fluoro-4-((pyridin-2-carbonyl)-amino)-phenyl)-4-acetoxy-pyrrolidine

→

trans-1-(4-acetoxy-2-(6-(4-methanesulfonyl-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone

용매

ethyl acetate

dimethylformamide

반응 조건

후처리

1. 1
   기타the reaction liquid
2. 2
   기타the reaction liquid
3. 3
   workup.STIRRINGwas stirred at 90° C. for 5 hours
4. 4
   기타The reaction liquid
5. 5
   세척washed with water and saturated saline in order
6. 6
   건조dried with anhydrous sodium sulfate
7. 7
   기타The solvent was evaporated away under reduced pressure
8. 8
   기타to obtain the entitled compound as a yellow oily substance

실험 절차

10 mg of 4-methanesulfonyl-phenol and 20 mg of cesium carbonate were added to a dimethylformamide (0.5 ml) solution of 21 mg of trans-1-acetyl-2-(5-nitro-2-fluoro-4-((pyridin-2-carbonyl)-amino)-phenyl)-4-acetoxy-pyrrolidine, and the reaction liquid was stirred at 90° C. for 1 hour. 100 mg of tin(II) chloride dihydrate was added to it, and the reaction liquid was stirred at 90° C. for 5 hours. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound as a yellow oily substance.

출처