반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:17]1[C:22]([O:23][CH2:24][CH3:25])=[CH:21][CH:20]=[CH:19][N:18]=1>C(Cl)Cl>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH3:15])[C:17]2[C:22]([O:23][CH2:24][CH3:25])=[CH:21][CH:20]=[CH:19][N:18]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1참가 물질
4
실험 절차
A mixture of 1-benzyl-4-(methylamino)piperidine (EXAMPLE 9, 2.92 g) and 2-bromo-3-ethoxypyridine (EXAMPLE 69, 1.44 g) is stirred at 160°-165° in a sealed tube for 2 days, diluted with methylene chloride (50 ml), washed with water (10 ml) and saline (10 ml), dried over sodium sulfate, and concentrated under reduced pressure. The residue is chromatographed on silica gel (230-400 mesh, 300 g; eluting with a gradient of ethyl acetate/hexane (10/90-50/50)) to give the title compound, C,H,N: Anal. Calcd for C20H27N3O1 : C=73.81, H=8.36, N=12.91-found: C=73.59, H=8.37, N=12.83.
후처리
- washwashed with water (10 ml) and saline (10 ml)
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue is chromatographed on silica gel (230-400 mesh, 300 g
- washeluting with a gradient of ethyl acetate/hexane (10/90-50/50))
출처 및 근거
- ORD 기록
- ord-f46c67e942b3493db6a54f5c40fb808f
- 출처 데이터셋
- uspto-grants-1999_02
- 특허 번호
- US05866589
연결된 노트
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