Methanol → 1,3-Diacetoxyacetone

HRID 356808

反応式

HRID 356808 の反応式
C1O[C:5]([OH:9])([CH2:7][OH:8])[CH2:4][O:3][C:2]1([OH:12])[CH2:10]O.[C:13](OC(=O)C)(=[O:15])[CH3:14].CO>CN(C1C=CN=CC=1)C.N1C=CC=CC=1>[C:13]([O:8][CH2:7][C:5]([CH2:4][O:3][C:2](=[O:12])[CH3:10])=[O:9])(=[O:15])[CH3:14]

参加物

6

反応物 3

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 4180364Dihydroxyacetone dimer

生成物 1

HCID 2434181,3-Diacetoxyacetone

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

Under an atmosphere of argon, 90 g of 1,3-dihydroxyacetone dimer and 250 mg of 4-(N,N-dimethylamino)pyridine were dissolved in 250 ml of pyridine. To the resulting solution, 225 ml of acetic anhydride was added droopowise at room temperature over 1 hour. After the resulting liquid was stirred at room temperature for 30 minutes, thereto was added 50 ml of methanol and the resulting liquid was further stirred at room temperature for 30 minutes. The solvent was removed under reduced pressure and the residue was subjected to a recrystallization from ether-petroleum ether to give 190 g of the desired compound.

後処理

  1. stirringthe resulting liquid was further stirred at room temperature for 30 minutes
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was subjected to a recrystallization from ether-petroleum ether

出典と根拠

ORDレコード
ord-33d87c0372054796ae65535c31a4f149
出典データセット
uspto-grants-1998_11
特許番号
US05840553

関連ノート

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