Ammonium formate → 4-(1-Acetylpiperidin-4-yl)furo[3,2-c]pyridine
반응식
[C:1]([N:4]1[CH2:9][CH:8]=[C:7]([C:10]2[C:15]3[CH:16]=[CH:17][O:18][C:14]=3[CH:13]=[CH:12][N:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].C([O-])=O.[NH4+]>CO.[Pd]>[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]2[C:15]3[CH:16]=[CH:17][O:18][C:14]=3[CH:13]=[CH:12][N:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]참가 물질
5
실험 절차
0.7 g of Pd/C (10%) is added to a solution of 3.4 g of the product obtained in Step C and 4.4 g of ammonium formate in 150 ml of anhydrous methanol under a stream of argon. After refluxing for 45 minutes, the reaction mixture is cooled, 4.4 g of ammonium formate and 0.2 g of Pd/C (10%) are added, and the reaction mixture is then heated at reflux for 30 minutes. After returning to ambient temperature, filtration over Celite and concentration under reduced pressure, the residue is taken up in water and then extracted with dichloromethane. The expected product is isolated by extraction, drying, filtration and concentration under reduced pressure.
후처리
- temperatureAfter refluxing for 45 minutes
- temperaturethe reaction mixture is cooled
- temperaturethe reaction mixture is then heated
- temperatureat reflux for 30 minutes
- customAfter returning to ambient temperature
- filtrationfiltration
- concentrationover Celite and concentration under reduced pressure
- extractionextracted with dichloromethane
출처 및 근거
- ORD 기록
- ord-b0a5f0e040c14630a5e0b2bf9cefc1c3
- 출처 데이터셋
- uspto-grants-2002_11
- 특허 번호
- US06486171B2
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