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

HRID 228929

반응식

HRID 228929 반응식
[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

참가 물질

5

반응물 2

HCID 83002-MethoxypropeneHCID 78432Trimethylolmethane

생성물 1

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

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-286338b454554e4489efeb880c1dd36b
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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