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

HRID 1987762ノート

反応式

HRID 1987762 の反応式
[NH:1]1[C:5]([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:4][CH:3]=[N: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]([C:5]5[NH:1][N:2]=[CH:3][CH:4]=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 231183091-(4-1H-pyrazol-5-ylphenyl)-piperazineHCID 688444542,4,6,7-Tetramethyl-5-nitrodihydrobenzofuran-2-carboxylic acid

生成物 1

HCID 68845480(+/-)-(5-Nitro-2,4,6,7-tetramethyldihydrobenzofuran-2-yl)-[4-(4-1h-pyrazol-5-ylphenyl)-piperazin-1-yl]carboxamide収率 90.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8471Triethylamine溶媒

実験手順

To 0.38 g of 1-(4-1H-pyrazol-5-ylphenyl)-piperazine and 0.4 g of 2,4,6,7-tetramethyl-5-nitrodihydrobenzofuran-2-carboxylic acid, 0.35 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, 0.25 g of 1-hydroxybenzotriazole hydrochloride and 0.19 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 then the resulting crystal was dried to obtain 0.65 g of the objective compound.

後処理

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

出典と根拠

ORDレコード
ord-41996fa04e8343d4bc13a543273b67dc
出典データセット
uspto-grants-2009_06
特許番号
US07553837B2

反応ノート

読み込み中…