Triethylamine → HCID 18917528、化合物

HRID 1290943

反応式

HRID 1290943 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[CH:21]=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1.[CH3:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[CH2:31][C:32](Cl)=[O:33].C(N(CC)CC)C>ClCCl>[CH:23]1[CH:22]=[CH:21][N:13]2[CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[N:10]([C:8]([C:5]3[CH:4]=[CH:3][C:2]([NH:1][C:32](=[O:33])[CH2:31][C:26]4[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=4[CH3:24])=[N:7][CH:6]=3)=[O:9])[CH2:11][C:12]=12

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2760632o-Tolyl-acetyl chlorideHCID 1891750110, 11-dihydro-10-(6-amino-3-pyridinylcarbonyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

生成物 1

HCID 18917528HCID 18917528、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2.0 mmol of 10,11-dihydro-10-(6-amino-3-pyridinylcarbonyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 2.1 mmol of 2-methylbenzeneacetyl chloride and 5 mmol of triethylamine in 10 ml of dichloromethane is stirred under argon at room temperature for 16 hours. The solvent is removed under vacuum and the residue partitioned between 50 ml of ethyl acetate and 25 ml of water. The organic layer is separated, washed with H2O, 1N NaHCO3, brine and dried (Na2SO4). The solvent is removed and the residue chromatographed on silica gel with ethyl acetate-hexane as solvent to give the product as a solid.

後処理

  1. customThe solvent is removed under vacuum
  2. customthe residue partitioned between 50 ml of ethyl acetate and 25 ml of water
  3. customThe organic layer is separated
  4. washwashed with H2O, 1N NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. customThe solvent is removed
  7. customthe residue chromatographed on silica gel with ethyl acetate-hexane as solvent

出典と根拠

ORDレコード
ord-78c2d3ccbabc42dbb5d01c81da310956
出典データセット
uspto-grants-1998_05
特許番号
US05753648

関連ノート

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