Succinic anhydride → HCID 86631996、化合物

HRID 1971638ノート

反応式

HRID 1971638 の反応式
[CH3:1][C@H:2]1[C@:10]2([OH:24])[C@H:11]3[C@:16]([OH:22])([CH2:17][C:18]([CH2:20][OH:21])=[CH:19][C@H:9]2[C@@H:5]2[C:6]([CH3:8])([CH3:7])[C@:4]2([O:25][C:26]([CH3:28])=[O:27])[CH2:3]1)[C:14](=[O:15])[C:13]([CH3:23])=[CH:12]3.[C:29]1(=[O:35])[O:34][C:32](=[O:33])[CH2:31][CH2:30]1.CN(C1C=CC=CN=1)C>ClCCl>[CH3:1][C@H:2]1[C@:10]2([OH:24])[C@H:11]3[C@:16]([OH:22])([CH2:17][C:18]([CH2:20][OH:21])=[CH:19][C@H:9]2[C@@H:5]2[C:6]([CH3:7])([CH3:8])[C@:4]2([O:25][C:26]([CH3:28])=[O:27])[CH2:3]1)[C:14](=[O:15])[C:13]([CH3:23])=[CH:12]3.[C:29]([O-:34])(=[O:35])[CH2:30][CH2:31][C:32]([O-:15])=[O:33]

参加物

5

反応物 3

HCID 7922Succinic anhydrideHCID 218852-DimethylaminopyridineHCID 454217Prostratin, PKC activator

生成物 1

HCID 86631996HCID 86631996、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Prostratin (1390 mg, 1 mmol) and succinic anhydride (120 mg, 1.2 mmol) were dissolved in dichloromethane (20 ml). DMAP (dimethylaminopyridine) at 50 mg was added under stirring and then stirred at room temperature for overnight. The solvent was evaporated and the residue subjected to chromatography on silica gel column (50 mg) with gradient of petroleum ether (60-90° C.) and acetone as eluent to give a fraction of pure prostratin succinate (Scheme (1), product 1) and another fraction containing a mixture of prostratin and prostratin succinate.

後処理

  1. stirringstirred at room temperature for overnight
  2. customThe solvent was evaporated
  3. customsubjected to chromatography on silica gel column (50 mg) with gradient of petroleum ether (60-90° C.) and acetone as eluent

出典と根拠

ORDレコード
ord-7f02a4eecc364646950c4c9efdfc7117
出典データセット
uspto-grants-2013_04
特許番号
US08431612B2

反応ノート

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