Ethylenediamine → Glycyrrhetinic acid ethylenediamine

HRID 705059

反応式

HRID 705059 の反応式
[CH3:1][C@@:2]12[CH2:24][CH2:23][C@:22]3([CH3:25])[C:8](=[CH:9][C:10]([C@H:12]4[C@@:21]3([CH3:26])[CH2:20][CH2:19][C@@H:18]3[C@:13]4([CH3:54])[CH2:14][CH2:15][C@H:16]([O:29][C@H:30]4[O:35][C@H:34]([C:36]([OH:38])=[O:37])[C@@H:33]([OH:39])[C@H:32]([OH:40])[C@H:31]4[O:41][C@@H:42]4[O:47][C@H:46]([C:48]([OH:50])=[O:49])[C@@H:45]([OH:51])[C@H:44]([OH:52])[C@H:43]4[OH:53])[C:17]3([CH3:28])[CH3:27])=[O:11])[C@@H:7]1[CH2:6][C@:5]([C:56]([OH:58])=[O:57])([CH3:55])[CH2:4][CH2:3]2.[CH2:59]([NH2:62])[CH2:60][NH2:61].C1(N=C=NC2CCCCC2)CCCCC1>CN(C=O)C>[CH3:1][C@@:2]12[CH2:24][CH2:23][C@:22]3([CH3:25])[C:8](=[CH:9][C:10]([C@H:12]4[C@@:21]3([CH3:26])[CH2:20][CH2:19][C@@H:18]3[C@:13]4([CH3:54])[CH2:14][CH2:15][C@H:16]([O:29][C@H:30]4[O:35][C@H:34]([C:36]([OH:38])=[O:37])[C@@H:33]([OH:39])[C@H:32]([OH:40])[C@H:31]4[O:41][C@@H:42]4[O:47][C@H:46]([C:48]([OH:50])=[O:49])[C@@H:45]([OH:51])[C@H:44]([OH:52])[C@H:43]4[OH:53])[C:17]3([CH3:27])[CH3:28])=[O:11])[C@@H:7]1[CH2:6][C@:5]([C:56]([OH:58])=[O:57])([CH3:55])[CH2:4][CH2:3]2.[CH2:59]([NH2:62])[CH2:60][NH2:61]

参加物

5

反応条件

温度
0 °C

実験手順

To N,N′-dimethylformamide (10 mL) were added glycyrrhetinic acid (1.0 mmol, 0.474 g) and ethylenediamine (30.0 mmol, 1.8 g, 2.0 mL). To the obtained solution were added dicyclohexyl carbodiimide (1.2 mmol, 0.247 g) and 4-N,N′-dimethylaminopyridine (catalytic amount) at 0° C. The mixture was stirred for 0.5-1 hour at 0° C. and then refluxed for further 12-48 hours. The resultant solution was filtered. To the filtrate was dropwise added diethyl ether. The precipitate was recovered and dried under vacuum to give glycyrrhetinic acid-ethylenediamine (yield=92%).

後処理

  1. temperaturerefluxed for further 12-48 hours
  2. filtrationThe resultant solution was filtered
  3. customThe precipitate was recovered
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-00b53f56056e4296abd143e2b0378110
出典データセット
uspto-grants-2015_11
特許番号
US09173852B2

関連ノート

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