Water → 5-Benzyloxymethyl-2,2-dimethyl-5-ethyl-1,3-dioxane

HRID 2372420

반응식

HRID 2372420 반응식
[CH3:1][C:2]1([CH3:12])[O:7][CH2:6][C:5]([CH2:10][CH3:11])([CH2:8][OH:9])[CH2:4][O:3]1.[H-].[Na+].[CH2:15](Cl)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.O>O1CCCC1>[CH2:15]([O:9][CH2:8][C:5]1([CH2:10][CH3:11])[CH2:4][O:3][C:2]([CH3:12])([CH3:1])[O:7][CH2:6]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7503Benzyl ChlorideHCID 24758Sodium hydrideHCID 118161521,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl-

생성물 1

HCID 199044005-Benzyloxymethyl-2,2-dimethyl-5-ethyl-1,3-dioxane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2,2-Dimethyl-5-ethyl-5-hydroxymethyl-1,3-dioxane (10 g.) was added to a stirred suspension of sodium hydride (2.4 g., 50% dispersion in oil) in dry tetrahydrofuran (80 ml.) The mixture was refluxed with stirring for one hour. Benzyl chloride (9.2 ml.) was added and the mixture was refluxed with stirring for three hours. the mixture was poured into water and the aqueous mixture was extracted with ether. The ethereal extract was washed with water, dried over anhydrous magnesium sulphate and evaporated in vacuo. 5-Benzyloxymethyl-2,2-dimethyl-5-ethyl-1,3-dioxane was obtained as a pale brown oil (15 g.) and was used without further purification.

후처리

  1. temperaturewas refluxed
  2. temperaturethe mixture was refluxed
  3. stirringwith stirring for three hours
  4. extractionthe aqueous mixture was extracted with ether
  5. extractionThe ethereal extract
  6. washwas washed with water
  7. dry with materialdried over anhydrous magnesium sulphate
  8. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-4df1e1f96fc046e49e70467d5c965774
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05098929

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