Methyl morpholine oxide → HCID 22926893、化合物

HRID 1985292ノート

反応式

HRID 1985292 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([O:18][CH:19]([CH3:21])[CH3:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C[N+]1([O-])CCOCC1>ClCCl.[Ru]([O-])(=O)(=O)=O.C([N+](CCC)(CCC)CCC)CC>[CH:2]([C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([O:18][CH:19]([CH3:20])[CH3:21])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10])=[O:1]

参加物

5

反応物 2

HCID 82029Methyl morpholine oxideHCID 22494341HCID 22494341、化合物

生成物 1

HCID 22926893HCID 22926893、化合物収率 95.3%

試薬・触媒・溶媒 2

HCID 178419074HCID 178419074、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

826 mg of Ethyl 3-[3-(hydroxymethyl)-4-methoxyphenyl]-2-isopropoxypropanoate was dissolved in 20 ml of dichloromethane, and 390 mg of N-methylmorpholine N-oxide, 1.4 g of molecular sieve 4A and 49 mg of tetrapropylammonium perruthenate were added, and the mixture was stirred at room temperature overnight. The reaction mixture was filtered through Celite, the filtrate was concentrated, and the residue was purified by silica gel column chromatography, to give 782 mg of the title compound in the 5:1→2:1 hexane-ethyl acetate fraction.

後処理

  1. filtrationThe reaction mixture was filtered through Celite
  2. concentrationthe filtrate was concentrated
  3. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-841fd412c5b9445dac495fe481d7264f
出典データセット
uspto-grants-2009_06
特許番号
US07544835B2

反応ノート

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