MAGNESIUM SILICATE (synthetic) → Betulone Aldehyde

HRID 414903ノート

反応式

HRID 414903 の反応式
[O-][Si]([O-])=O.[Mg+2].C([O-])(=O)C.[Na+].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.[CH3:22][C:23]([C@H:25]1[C@@H:29]2[C@@H:30]3[C@@:43]([CH3:46])([CH2:44][CH2:45][C@@:28]2([CH2:52][OH:53])[CH2:27][CH2:26]1)[C@@:42]1([CH3:47])[C@@H:33]([C@:34]2([CH3:51])[C@@H:39]([CH2:40][CH2:41]1)[C:38]([CH3:49])([CH3:48])[C@@H:37]([OH:50])[CH2:36][CH2:35]2)[CH2:32][CH2:31]3)=[CH2:24]>C(Cl)Cl>[CH3:24][C:23]([C@H:25]1[C@@H:29]2[C@H:30]3[C@@:43]([CH3:46])([CH2:44][CH2:45][C@@:28]2([CH:52]=[O:53])[CH2:27][CH2:26]1)[C@:42]1([CH3:47])[CH2:41][CH2:40][C@H:39]2[C:38]([CH3:49])([CH3:48])[C:37](=[O:50])[CH:36]=[CH:35][C@:34]2([CH3:51])[C@H:33]1[CH2:32][CH2:31]3)=[CH2:22]

参加物

6

反応物 4

HCID 61680MAGNESIUM SILICATE (synthetic)HCID 72326BetulinHCID 517045Sodium AcetateHCID 178418287HCID 178418287、化合物

生成物 1

HCID 44559212Betulone Aldehyde収率 75%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of freshly activated powdered 4A molecular sieves (1.2 g), celite (1.2 g), florisil (1.2 g), sodium acetate (500 mg) and pyridinium chlorochromate (1.2 g) in CH2Cl2 (25 mL) add betulin (500 mg). The mixture is to be stirred for 2 hrs, and then filtered through a short column of silica gel. The filtrate is evaporated in vacuo. The residue is then subjected to column chromatography to afford betulone aldehyde (370 mg) as white solid.

後処理

  1. additionTo a suspension
  2. filtrationfiltered through a short column of silica gel
  3. customThe filtrate is evaporated in vacuo

出典と根拠

ORDレコード
ord-1845d7038c7d4ac7a5d33fed45637898
出典データセット
uspto-grants-2012_01
特許番号
US08088757B2

反応ノート

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