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

HRID 362396ノート

反応式

HRID 362396 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-96b2838ef96948b3ab417d43510bfc3a
出典データセット
uspto-grants-1999_02
特許番号
US05869483

反応ノート

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