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1-Benzyl-1,2-dihydropyridine-4-carboxamide → HCID 18634675, 화합물

HRID 2051302
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HRID 2051302 반응식
[I-].[I-].[CH3:3][N+:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([O:12][C:13]2[CH:30]=[CH:29][C:28]3[C@@H:27]4[C@H:18]([C@H:19]5[C@@:23]([CH2:25][CH2:26]4)([CH3:24])[C@@H:22]([O:31][C:32]([C:34]4[CH:35]=[N+:36]([CH3:40])[CH:37]=[CH:38][CH:39]=4)=[O:33])[CH2:21][CH2:20]5)[CH2:17][CH2:16][C:15]=3[CH:14]=2)=[O:11])[CH:5]=1.C1(CN2C=CC(C(N)=O)=CC2)C=CC=CC=1>C(#N)C.C(Cl)Cl>[CH3:3][N:4]1[CH:9]=[CH:8][CH2:7][C:6]([C:10]([O:12][C:13]2[CH:30]=[CH:29][C:28]3[C@@H:27]4[C@H:18]([C@H:19]5[C@@:23]([CH2:25][CH2:26]4)([CH3:24])[C@@H:22]([O:31][C:32]([C:34]4[CH2:39][CH:38]=[CH:37][N:36]([CH3:40])[CH:35]=4)=[O:33])[CH2:21][CH2:20]5)[CH2:17][CH2:16][C:15]=3[CH:14]=2)=[O:11])=[CH:5]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 132279601-Benzyl-1,2-dihydropyridine-4-carboxamideHCID 13731100HCID 13731100, 화합물

생성물 1

HCID 18634675HCID 18634675, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

One gram (1.31 mmol) of the product of Example 71 was dissolved in 100 mL of dry acetonitrile. To that solution, which was flushed with nitrogen, 0.28 g (1.31 mmol) of 1-(phenylmethyl)-4-(aminocarbonyl)-1,2-dihydropyridine was added, and the reaction mixture was stirred at 0° C. for 1 hour. Removal of the solvent under reduced pressure afforded a solid, which was suspended in methylene chloride and removed by filtration. The filtrate was chromatographed several times on a neutral alumina column prepared with methylene chloride. Purification and evaporation of the solvent in vacuo gave a solid foam. The product had the formula ##STR104## as confirmed by UV, NMR and elemental analyses.

후처리

  1. additionwas added
  2. customRemoval of the solvent under reduced pressure
  3. customafforded a solid, which
  4. customremoved by filtration
  5. customThe filtrate was chromatographed several times on a neutral alumina column
  6. customprepared with methylene chloride
  7. customPurification and evaporation of the solvent in vacuo
  8. customgave a solid foam

출처 및 근거

ORD 기록
ord-0a05ad1669804cbc9e1d3cefbb1deb91
출처 데이터셋
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05017566

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