Triethylamine → N-[4-(6,7-Dihydro-dibenzo[b,d]azepine-5-carbonyl)-phenyl]-2-methyl-benzamide

HRID 355899노트

반응식

HRID 355899 반응식
[NH2:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([N:8]2[CH2:14][CH2:13][C:12]3[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=3[C:10]3[CH:19]=[CH:20][CH:21]=[CH:22][C:9]2=3)=[O:7])=[CH:4][CH:3]=1.C(N([CH2:30][CH3:31])CC)C>ClCCl.C(OCC)(=O)C>[CH:19]1[C:10]2[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13][CH2:14][N:8]([C:6]([C:5]3[CH:23]=[CH:24][C:2]([NH:1][C:6](=[O:7])[C:5]4[CH:4]=[CH:3][CH:2]=[CH:24][C:30]=4[CH3:31])=[CH:3][CH:4]=3)=[O:7])[C:9]=2[CH:22]=[CH:21][CH:20]=1

참가 물질

5

반응물 2

HCID 8471TriethylamineHCID 538444955-(4-Aminobenzoyl)-6,7-dihydro-5H-dibenz[b,d]azepine

생성물 1

HCID 44212554N-[4-(6,7-Dihydro-dibenzo[b,d]azepine-5-carbonyl)-phenyl]-2-methyl-benzamide수율 130.8%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 0.10 g of 5-(4-aminobenzoyl)-6,7-dihydro-5H-dibenz[b,d]azepine, 0.10 g of triethylamine in 1 ml of dichloromethane is stirred at room temperature for 6 hours. The mixture is diluted with 6 ml of ethyl acetate and the solution washed with 1N HCl, 1N NaOH, brine and dried (Na2SO4). The solvent is removed and the solid purified by chromatography on thick layer silica gel plates with the solvent ethyl acetate-hexane (1:1) to give 90 mg of a pale yellow solid.

후처리

  1. washthe solution washed with 1N HCl, 1N NaOH, brine
  2. dry with materialdried (Na2SO4)
  3. customThe solvent is removed
  4. customthe solid purified by chromatography on thick layer silica gel plates with the solvent ethyl acetate-hexane (1:1)

출처 및 근거

ORD 기록
ord-24882e66595342029a59a41845983702
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834461

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