Water → 5-(1,3-Dioxan-2-yl)-1-methyl-1H-imidazole

HRID 84358

反応式

HRID 84358 の反応式
[CH3:1][N:2]1[C:6]([CH:7]=[O:8])=[CH:5][N:4]=[CH:3]1.[CH2:9](O)[CH2:10][CH2:11][OH:12].CC1(C)C2(CS(O)(=O)=O)C(CC1CC2)=O.O>C1(C)C=CC=CC=1.C(Cl)Cl>[O:8]1[CH2:9][CH2:10][CH2:11][O:12][CH:7]1[C:6]1[N:2]([CH3:1])[CH:3]=[N:4][CH:5]=1

参加物

7

反応物 4

HCID 962WaterHCID 104421,3-PropanediolHCID 18462Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)-HCID 5735921-methyl-1H-imidazole-5-carbaldehyde

生成物 1

HCID 579196325-(1,3-Dioxan-2-yl)-1-methyl-1H-imidazole

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-methyl-1H-imidazole-5-carbaldehyde (2.9 g, 26.3 mmol) in toluene (20 mL) was added propane-1,3-diol (4.01 g, 52.7 mmol) and CSA (0.306 g, 1.317 mmol) and the reaction mixture was heated to reflux with azeotropic removal of the evolved water for 24 hours. The reaction mixture was cooled to RT, diluted with DCM and washed with NaHCO3 solution.

後処理

  1. temperaturethe reaction mixture was heated
  2. washwashed with NaHCO3 solution

出典と根拠

ORDレコード
ord-e7428bd3e70b498dbb8013ec465cb6e1
出典データセット
uspto-grants-2014_09
特許番号
US08846927B2

関連ノート

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