Water → HCID 19373306、化合物

HRID 1197376ノート

反応式

HRID 1197376 の反応式
[OH:1][CH2:2][C:3]1([CH2:11][OH:12])[CH2:8][O:7][C:6]([CH3:10])([CH3:9])[O:5][CH2:4]1.[H-].[Na+].[CH2:15](I)[CH3:16].O>CN(C)C=O>[CH3:10][C:6]1([CH3:9])[O:5][CH2:4][C:3]([CH2:11][O:12][CH2:15][CH3:16])([CH2:2][OH:1])[CH2:8][O:7]1

参加物

6

反応物 4

HCID 962WaterHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 373708NSC650609

生成物 1

HCID 19373306HCID 19373306、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a stirred solution of 5,5-di-(hydroxymethyl)-2,2-dimethyl-1,3-dioxane (5.0 g) (Beilstein 19, II, 93) in dry dimethylformamide (50 ml) under nitrogen, at 20°, was added sodium hydride (0.68 g, 80% dispersion in oil). The mixture was stirred at 80° for 2 hours and cooled. Ethyl iodide (4.4 g) in dry dimethylformamide (40 ml) was added and the mixture was heated at 110° for 3 hours. The mixture was cooled and poured into water. The aqueous mixture was extracted with diethyl ether. The ethereal extracts were washed with brine, dried over anhydrous magnesium sulphate and evaporated in vacuo. 2,2-Dimethyl-5-ethoxymethyl-5-hydroxymethyl-1,3-dioxane was obtained as a pale yellow oil (1.2 g) and was used without further purification.

後処理

  1. temperaturecooled
  2. temperaturethe mixture was heated at 110° for 3 hours
  3. temperatureThe mixture was cooled
  4. extractionThe aqueous mixture was extracted with diethyl ether
  5. washThe ethereal extracts were washed with brine
  6. dry with materialdried over anhydrous magnesium sulphate
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-b5a1b2e458c44ca5ac34c337b2034a59
出典データセット
uspto-grants-1992_05
特許番号
US05116862

反応ノート

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