2-Methoxypropene → (2,2-Dimethyl-1,3-dioxan-5-yl)methanol

HRID 228929

反応式

HRID 228929 の反応式
[CH3:1][O:2][C:3]([CH3:5])=[CH2:4].[OH:6][CH2:7][CH:8](CO)[CH2:9][OH:10]>CN(C)C=O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH3:4][C:3]1([CH3:5])[O:6][CH2:7][CH:8]([CH2:9][OH:10])[CH2:1][O:2]1

参加物

5

反応物 2

HCID 83002-MethoxypropeneHCID 78432Trimethylolmethane

生成物 1

HCID 3584869(2,2-Dimethyl-1,3-dioxan-5-yl)methanol収率 55%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-methoxypropene (1 g) in N,N-dimethylformamide (150 ml) was added to 2-(hydroxymethyl)-1,3-propanediol (500 mg). p-Toluenesulfonic acid (10 mg) was added thereto, and the mixture was stirred at room temperature overnight. The solvent was removed by distillation under the reduced pressure, water was added to the residue, and the mixture was extracted with n-butanol. The n-butanol layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using hexane-acetone to give (2,2-dimethyl[1,3]dioxan-5-yl)-methanol (378 mg, yield 55%).

後処理

  1. customThe solvent was removed by distillation under the reduced pressure, water
  2. additionwas added to the residue
  3. extractionthe mixture was extracted with n-butanol
  4. washThe n-butanol layer was then washed with water
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. customThe solvent was removed by distillation under the reduced pressure
  7. customthe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-286338b454554e4489efeb880c1dd36b
出典データセット
uspto-grants-2009_07
特許番号
US07560558B2

関連ノート

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