Water → 2,2-Dimethyl-5-ethyl-5-hydroxymethyl-1,3-dioxane methylsulphonate

HRID 704128

反応式

HRID 704128 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][C:7]1([CH3:17])[O:12][CH2:11][C:10]([CH2:15][CH3:16])([CH2:13][OH:14])[CH2:9][O:8]1.O>N1C=CC=CC=1>[CH3:1][S:2]([OH:4])(=[O:8])=[O:3].[CH3:6][C:7]1([CH3:17])[O:8][CH2:9][C:10]([CH2:15][CH3:16])([CH2:13][OH:14])[CH2:11][O:12]1

参加物

5

反応物 3

HCID 962WaterHCID 31297Methanesulfonyl chlorideHCID 118161521,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl-

生成物 1

HCID 200755932,2-Dimethyl-5-ethyl-5-hydroxymethyl-1,3-dioxane methylsulphonate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Methanesulphonyl chloride (15 ml.) was added dropwise to a stirred solution of 2,2-dimethyl-5-ethyl-5-hydroxymethyl-1,3-dioxane 1 (33.0 g) in dry pyridine (100 ml.) at 0°. The mixture was stirred for two hours at room temperature and then poured into water. The aqueous mixture was extracted with ether. The ethereal extracts were washed with water, dried over anhydrous magnesium sulphate and evaporated in vacuo. 2,2-Dimethyl-5-ethyl-5-hydroxymethyl-1,3-dioxane methane sulphonate was obtained as a colourless oil (39 g.) which solidified on standing. The compound was used without further purification.

後処理

  1. extractionThe aqueous mixture was extracted with ether
  2. washThe ethereal extracts were washed with water
  3. dry with materialdried over anhydrous magnesium sulphate
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-8084b5d0d46c477d9685028d329a148e
出典データセット
uspto-grants-1991_01
特許番号
US04985582

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