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Triethylamine → HCID 15907546、化合物

HRID 459741
ノート
印刷プレビュー

反応式

HRID 459741 の反応式
C[N:2]1CCNCC1C1C=CC(N)=CC=1.O[C:16]1[C:24]2N=N[NH:21][C:20]=2[CH:19]=[CH:18][CH:17]=1.Cl.CN(C)CCCN=C=NCC.[CH2:37]([N:39]([CH2:42][CH3:43])[CH2:40][CH3:41])C.[N+:44]([C:47]1[CH:52]=[CH:51][C:50]([CH2:53][CH2:54][CH2:55][C:56]([OH:58])=O)=[CH:49][CH:48]=1)([O-:46])=[O:45]>ClCCl.O>[N+:44]([C:47]1[CH:52]=[CH:51][C:50]([CH2:53][CH2:54][CH2:55][C:56]([NH:2][C:17]2[CH:16]=[CH:24][C:20]([N:21]3[CH2:43][CH2:42][N:39]([CH3:37])[CH2:40][CH2:41]3)=[CH:19][CH:18]=2)=[O:58])=[CH:49][CH:48]=1)([O-:46])=[O:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8471TriethylamineHCID 797114-(4-Nitrophenyl)butyric acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 68579243HCID 68579243、化合物HCID 178418300HCID 178418300、化合物

生成物 1

HCID 15907546HCID 15907546、化合物収率 84%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

4-(N-methylpiperazinyl)aniline (0.5 g; 2.6 mmol), hydroxybenzotriazole (0.39 g; 2.86 mmol), 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (1.1 g; 5.7 mmol) and triethylamine (0.8 ml; 5.7 mmol) are added to a solution of 0.55 g (2.6 mmol) of 4-(4-nitrophenyl)butanoic acid in dichloromethane (30 ml). The reaction medium is stirred for 16 hours at ambient temperature, then the medium is diluted with 15 ml of water and the product is extracted with dichloromethane. The organic phase is dried over sodium sulphate followed by filtering and concentrating under vacuum and the residue is purified on a silica column (eluent: CH2Cl2/EtOH: 4/1). A clear oil is obtained with a yield of 84% (0.84 g).

後処理

  1. extractionthe product is extracted with dichloromethane
  2. dry with materialThe organic phase is dried over sodium sulphate
  3. filtrationby filtering
  4. concentrationconcentrating under vacuum
  5. customthe residue is purified on a silica column (eluent: CH2Cl2/EtOH: 4/1)
  6. customA clear oil is obtained with a yield of 84% (0.84 g)

出典と根拠

ORDレコード
ord-b41610da23d04c1baa346187642f635e
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07196084B2

反応ノート

読み込み中…

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