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1-Hydroxybenzotriazole → N-(12-hydroxydodecyl)-6-(4-ethyl-1-piperazinyl)pyridine-3-carboxamide

HRID 1003306
ノート
印刷プレビュー

反応式

HRID 1003306 の反応式
[CH2:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]2[N:14]=[CH:13][C:12]([C:15]([O-:17])=O)=[CH:11][CH:10]=2)[CH2:5][CH2:4]1)[CH3:2].[K+].[NH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][OH:32].Cl.C(N=C=NCCCN(C)C)C.ON1C2C=CC=CC=2N=N1>C(Cl)Cl>[OH:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][NH:19][C:15]([C:12]1[CH:13]=[N:14][C:9]([N:6]2[CH2:5][CH2:4][N:3]([CH2:1][CH3:2])[CH2:8][CH2:7]2)=[CH:10][CH:11]=1)=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 518202012-Amino-1-dodecanolHCID 23663822Potassium 6-(4-ethyl-1-piperazinyl)pyridine-3-carboxylate

生成物 1

HCID 15462624N-(12-hydroxydodecyl)-6-(4-ethyl-1-piperazinyl)pyridine-3-carboxamide収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 4.07 g of potassium 6-(4-ethyl-1-piperazinyl)-pyridine-3-carboxylate and 3.00 g of 12-aminododecanol was added 50 ml of methylene chloride and then 2.86 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (WSCI) and 2.01 g of 1-hydroxybenzotriazole (HOBt) were added while stirring at room temperature. The mixture was stirred at room temperature for 15 hours. To the reaction solution were added water and diisopropyl ether and subsequent filtration and drying under reduced pressure afforded 5.67 g of the title compound as a crystal.

後処理

  1. stirringThe mixture was stirred at room temperature for 15 hours
  2. additionTo the reaction solution were added
  3. filtrationwater and diisopropyl ether and subsequent filtration
  4. customdrying under reduced pressure

出典と根拠

ORDレコード
ord-88bf458d576b487990051a158e02cd63
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06046201

反応ノート

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