Methanol → 1,3-Diacetoxyacetone

HRID 356808

반응식

HRID 356808 반응식
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]

참가 물질

6

반응물 3

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 4180364Dihydroxyacetone dimer

생성물 1

HCID 2434181,3-Diacetoxyacetone

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-33d87c0372054796ae65535c31a4f149
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840553

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