Ethylene glycol monoallyl ether → Allyl methanesulfonylethyl ether

HRID 379465

반응식

HRID 379465 반응식
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]

참가 물질

5

반응물 3

HCID 8116Ethylene glycol monoallyl etherHCID 31297Methanesulfonyl chlorideHCID 81531Diisopropylethylamine

생성물 1

HCID 57200585Allyl methanesulfonylethyl ether

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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 1M aqueous hydrochloric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to obtain allyl methanesulfonylethyl ether: Rf=0.80 (silica gel, 20% ethyl acetate/dichloromethane).

후처리

  1. temperatureCool in an ice-bath
  2. additionAdd dropwise
  3. extractionextract the reaction mixture with 1M 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 in vacuo

출처 및 근거

ORD 기록
ord-f637eb5c321945cd8647ddca66bb4db8
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297259B1

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