ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1,2-Ethanediamine, N1,N1,N2-trimethyl- → HCID 178501159、化合物

HRID 16717
ノート
印刷プレビュー

反応式

HRID 16717 の反応式
[CH3:1][O:2][C:3]([C@H:5]1[CH2:10][CH2:9][C@H:8]([C:11]([OH:13])=O)[CH2:7][CH2:6]1)=[O:4].ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C.[CH3:36][N:37]([CH3:42])[CH2:38][CH2:39][NH:40][CH3:41].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[CH3:36][N:37]([CH3:42])[CH2:38][CH2:39][N:40]([CH3:41])[C:11]([C@H:8]1[CH2:7][CH2:6][C@H:5]([C:3]([O:2][CH3:1])=[O:4])[CH2:10][CH2:9]1)=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 673381,2-Ethanediamine, N1,N1,N2-trimethyl-HCID 757711-HydroxybenzotriazoleHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 178501163HCID 178501163、化合物

生成物 1

HCID 178501159HCID 178501159、化合物収率 93.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Trans-4-(methoxycarbonyl)cyclohexanecarboxylic acid (8.84 g) obtained in Reference Example 1(2) is dissolved in chloroform (100 ml), and thereto are added 1-hydroxybenzotriazole (7.14 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (10.00 g) and N,N,N′-trimethylethylenediamine (5.33 g) under ice-cooling. The mixture is then stirred at room temperature for 4 hours. Saturated aqueous sodium hydrogen carbonate solution is poured to the reaction solution and the mixture is extracted with chloroform. The organic layer is washed with saturated brine and dried over sodium sulfate. The solvent is concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (eluent: chloroform/methanol/28% ammonia water=200/10/1) to give methyl trans-4-{[[2-(dimethylamino)ethyl](methyl)amino]carbonyl}-cyclohexanecarboxylate (11.98 g).

後処理

  1. temperaturecooling
  2. extractionthe mixture is extracted with chloroform
  3. washThe organic layer is washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationThe solvent is concentrated under reduced pressure
  6. customThe resulting residue is purified by silica gel column chromatography (eluent: chloroform/methanol/28% ammonia water=200/10/1)

出典と根拠

ORDレコード
ord-8b58af24ecdb470eb2de945d1ee82651
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07737161B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート