Ethylene glycol monoallyl ether → Allyl methanesulfonylethyl ether

HRID 609787

反応式

HRID 609787 の反応式
O[CH2:2][CH2:3][O:4][CH2:5][CH:6]=[CH2:7].C(N(C(C)C)CC)(C)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>ClCCl>[CH3:17][S:18]([CH2:2][CH2:3][O:4][CH2:5][CH:6]=[CH2:7])(=[O:20])=[O:19]

参加物

5

反応物 3

HCID 8116Ethylene glycol monoallyl etherHCID 31297Methanesulfonyl chlorideHCID 81531Diisopropylethylamine

生成物 1

HCID 57200585Allyl methanesulfonylethyl ether

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Combine allyl hydroxyethyl ether (1.02 g, 10 mmol), and diisopropylethylamine (4.0 mL, 23 mmol), and dichloromethane (20 mL). Cool in an ice-bath. Add dropwise, methanesulfonyl chloride (1.0 mL, 13 mmol). After 1.5 hours, extract the reaction mixture with 1 M aqueous hydrochloric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution. Dry the organic layer over Na2SO4, filter, and evaporate invacuo to obtain allyl methanesulfonylethyl ether: Rf =0.80 (silica gel, 20% ethyl acetate/dichloromethane).

後処理

  1. temperatureCool in an ice-bath
  2. additionAdd dropwise
  3. extractionextract the reaction mixture with 1 M aqueous hydrochloric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution
  4. dry with materialDry the organic layer over Na2SO4
  5. filtrationfilter
  6. customevaporate invacuo

出典と根拠

ORDレコード
ord-49773dd96dc142c1980df3ce4dd043d7
出典データセット
uspto-grants-1999_12
特許番号
US05998439

関連ノート

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