반응 #68070
ord-c8877660e778476d8db4c8cbf29f30e8
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반응 조건
후처리
- 1workup.ADDITIONwas added
- 2workup.STIRRINGstirred at 55-60° C. for 1 hour
- 3온도The mixture was cooled to the room temperature
- 4workup.WAITleft
- 5workup.WAITto stand for 2 nights
- 6기타The solvent was removed under reduced pressure, water
- 7workup.ADDITIONwas added
- 8workup.ADDITIONwas added
- 9기타the solvent was removed under reduced pressure
- 10workup.ADDITIONWater was added
- 11여과the resulting solid was filtered
실험 절차
To 2 mL of an ethanol solution containing 90 mg of ethyl 4-(3-(2-oxoquinoxalin-1(2H)-yl)propyl)-1-(2-(2-thienylthio)ethyl)piperidine-4-carboxylate, 0.5 mL of 20% aqueous sodium hydroxide solution was added and stirred at 55-60° C. for 5 hours. 0.5 mL of 20% aqueous sodium hydroxide solution and 0.5 mL of water were added at the same temperature, and stirred at 55-60° C. for 1 hour. The mixture was cooled to the room temperature, and left to stand for 2 nights. The solvent was removed under reduced pressure, water was added, adjusted to pH 6.5 with 6.0 mol/L hydrochloric acid, acetonitrile was added, and the solvent was removed under reduced pressure. Water was added, and the resulting solid was filtered to afford 35 mg of 4-(3-(2-oxoquinoxaline-1(2H)-yl)propyl)-1-(2-(2-thienylthio)ethyl)piperidine-4-carboxylic acid as a brown solid.