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

HRID 2372420

反応式

HRID 2372420 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4df1e1f96fc046e49e70467d5c965774
出典データセット
uspto-grants-1992_03
特許番号
US05098929

関連ノート

読み込み中…