Succinic anhydride → HCID 86631996、化合物

HRID 910470ノート

反応式

HRID 910470 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-3d8d2ec0faff42e695d38ac9c1c31cf7
出典データセット
uspto-grants-2011_09
特許番号
US08022103B2

反応ノート

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