Triethylamine → 4-[(6,7-Dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-5-ylcarbonyl)phenyl]-2-methyl-benzamide

HRID 1420025ノート

反応式

HRID 1420025 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].C([N:13](CC)CC)C.N[C:19]1[CH:40]=[CH:39][C:22]([C:23]([N:25]2[C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=3[N:29]3[CH:36]=[CH:37][CH:38]=[C:28]3[CH2:27][CH2:26]2)=[O:24])=[CH:21][CH:20]=1>C(Cl)Cl>[CH:35]1[C:30]2[N:29]3[CH:36]=[CH:37][CH:38]=[C:28]3[CH2:27][CH2:26][N:25]([C:23]([C:22]3[CH:21]=[CH:20][CH:19]=[CH:40][C:39]=3[C:9]3[CH:8]=[CH:7][C:3]([C:4]([NH2:13])=[O:5])=[C:2]([CH3:1])[CH:10]=3)=[O:24])[C:31]=2[CH:32]=[CH:33][CH:34]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 702762-Methylbenzoyl chlorideHCID 218371566,7-Dihydro-5-(4-aminobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine

生成物 1

HCID 867507754-[(6,7-Dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-5-ylcarbonyl)phenyl]-2-methyl-benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 5 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 7 mmol of triethylamine and 5 mmol of 6,7-dihydro-5-(4-aminobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine. The reaction mixture is washed with water, 2M citric acid, NaHCO3, and brine. The organic layer is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography on silica gel to give the desired product as a solid; mass spectrum (CI):422(M+H).

後処理

  1. washThe reaction mixture is washed with water, 2M citric acid, NaHCO3, and brine
  2. dry with materialThe organic layer is dried with Na2SO4
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customto give a solid which
  6. customis purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-3675bcc1bce143879259d6393c3da7e8
出典データセット
uspto-grants-1999_03
特許番号
US05889001

反応ノート

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