1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → (+/-)-(5-Nitro-2,4,6,7-tetramethyldihydrobenzofuran-2-yl)-[4-(4-imidazol-1-ylphenyl)-piperazin-1-yl]carboxamide

HRID 1987759ノート

反応式

HRID 1987759 の反応式
[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([N:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.C[C:19]1([C:34](O)=O)[CH2:23][CH:22]2[CH:24]([CH3:33])[C:25]([N+:30]([O-:32])=[O:31])=[C:26]([CH3:29])[C:27]([CH3:28])=[C:21]2[O:20]1.Cl.C[N:39]([CH3:48])CCCN=C=NCC.Cl.[OH:50]N1C2C=CC=CC=2N=N1>O.C(N(CC)CC)C>[N+:30]([C:25]1[CH:24]([CH3:33])[CH:22]2[CH2:23][C:19]([NH:39][C:48]([N:15]3[CH2:16][CH2:17][N:12]([C:9]4[CH:8]=[CH:7][C:6]([N:1]5[CH:5]=[CH:4][N:3]=[CH:2]5)=[CH:11][CH:10]=4)[CH2:13][CH2:14]3)=[O:50])([CH3:34])[O:20][C:21]2=[C:27]([CH3:28])[C:26]=1[CH3:29])([O-:32])=[O:31]

参加物

7

反応物 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 22729017HOBT hydrochlorideHCID 231182901-(4-(1H-imidazol-1-yl)phenyl)piperazineHCID 688444542,4,6,7-Tetramethyl-5-nitrodihydrobenzofuran-2-carboxylic acid

生成物 1

HCID 68849562(+/-)-(5-Nitro-2,4,6,7-tetramethyldihydrobenzofuran-2-yl)-[4-(4-imidazol-1-ylphenyl)-piperazin-1-yl]carboxamide収率 98.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8471Triethylamine溶媒

実験手順

To 0.43 g of 1-(4-imidazol-1-ylphenyl)-piperazine and 0.5 g of 2,4,6,7-tetramethyl-5-nitrodihydrobenzofuran-2-carboxylic acid, 0.44 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, 0.31 g of 1-hydroxybenzotriazole hydrochloride and 0.23 g of triethylamine were added, followed by stirring at room temperature for 24 hours. The reaction solution was poured into water and the precipitated crystal was removed by filtration and washed with water and ether, and then the resulting crystal was dried to obtain 0.88 g of the objective compound.

後処理

  1. customthe precipitated crystal was removed by filtration
  2. washwashed with water and ether
  3. customthe resulting crystal was dried

出典と根拠

ORDレコード
ord-7611fe4541e44aacb4103cfbf8a325b6
出典データセット
uspto-grants-2009_06
特許番号
US07553837B2

反応ノート

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