Triethylamine → N-[4-(4H-Furo[2,3-e]pyrrolo[1,2-a][1,4]-diazepin-10(9H)-ylcarbonyl)phenyl]-2-methyl benzamide

HRID 1420006

反応式

HRID 1420006 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(CC)CC)C.[NH2:18][C:19]1[CH:39]=[CH:38][C:22]([C:23]([N:25]2[C:31]3[O:32][CH:33]=[CH:34][C:30]=3[CH2:29][N:28]3[CH:35]=[CH:36][CH:37]=[C:27]3[CH2:26]2)=[O:24])=[CH:21][CH:20]=1>C(Cl)Cl>[O:32]1[C:31]2[N:25]([C:23]([C:22]3[CH:21]=[CH:20][C:19]([NH:18][C:4](=[O:5])[C:3]4[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=4[CH3:1])=[CH:39][CH:38]=3)=[O:24])[CH2:26][C:27]3[N:28]([CH:35]=[CH:36][CH:37]=3)[CH2:29][C:30]=2[CH:34]=[CH:33]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 702762-Methylbenzoyl chlorideHCID 540426559,10-Dihydro-10-(4-aminobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine

生成物 1

HCID 21837211N-[4-(4H-Furo[2,3-e]pyrrolo[1,2-a][1,4]-diazepin-10(9H)-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 1.1 mmol of 2-methylbenzoyl chloride in 10 ml of methylene chloride is added 1.5 mmol of triethylamine. To the mixture is added 1.1 mmol of 9,10-dihydro-10-(4-aminobenzoyl)-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine and the mixture is stirred for 5 hours. The reaction mixture is washed with water, 1N citric acid, NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography on silica gel with ethyl acetate-hexane as solvent to give the desired product as a solid.

後処理

  1. washThe reaction mixture is washed with water, 1N citric acid, NaHCO3, and brine
  2. dry with materialThe reaction mixture 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 with ethyl acetate-hexane as solvent

出典と根拠

ORDレコード
ord-103c6f2149334a29a62d756ecc5a154b
出典データセット
uspto-grants-1999_03
特許番号
US05889001

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