Water → 2-Methyl-2-nitro-1-(methoxymethoxy)propane

HRID 636736ノート

反応式

HRID 636736 の反応式
[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][OH:4].[Li+].[Br-].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.O.[CH3:24][O:25][CH2:26]OC>>[CH3:1][C:2]([N+:6]([O-:8])=[O:7])([CH3:5])[CH2:3][O:4][CH2:24][O:25][CH3:26]

参加物

6

実験手順

To a solution of 2-methyl-2-nitro-1-propanol (366.8 mg, 3.08 mmol) and LiBr (60.8 mg, 0.700 mmol) in dimethoxymethane (5 ml) was added p-toluenesulfonic acid hydrate (56.3 mg, 0.296 mmol) and stirred for 24 hours. The mixture was added to water and extracted three times with ethyl acetate and dried over MgSO4. The mixture was concentrated and purified by silica gel chromatography (hexane/ether=4/1) to give the title compound (382.7 mg; 76%).

後処理

  1. extractionextracted three times with ethyl acetate
  2. dry with materialdried over MgSO4
  3. concentrationThe mixture was concentrated
  4. custompurified by silica gel chromatography (hexane/ether=4/1)

出典と根拠

ORDレコード
ord-65625b631df84f3c80df010961eff1d7
出典データセット
uspto-grants-2001_02
特許番号
US06194461B1

反応ノート

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