Diethylene Glycol Monomethyl Ether → 2-(2-Methoxyethoxy)ethyl methanesulfonate

HRID 2200573

반응식

HRID 2200573 반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][OH:8].[CH3:9][S:10](Cl)(=[O:12])=[O:11]>C(Cl)Cl>[CH3:9][S:10]([O:8][CH2:7][CH2:6][O:5][CH2:4][CH2:3][O:2][CH3:1])(=[O:12])=[O:11]

참가 물질

4

반응물 2

HCID 8134Diethylene Glycol Monomethyl EtherHCID 31297Methanesulfonyl chloride

생성물 1

HCID 38156542-(2-Methoxyethoxy)ethyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-(2-methoxyethoxy)ethanol (300 mg, 2.5 mmol) in DCM (5 mL) was added methanesulfonyl chloride (370 mg, 2.6 mmol) dropwise at 0° C. After stirred at this temperature for 5 min, TEA (505 mg, 5.0 mmol) was added. It was stirred at room temperature overnight. The mixture was partitioned between DCM and water. The organic layers were combined, dried over sodium sulfate, filtered and concentrated to give a crude oil product, which was used without purification. Product tlc [petroleum ether/ethyl acetate [1:1) developed with iodine, Rf 0.5]

후처리

  1. stirringIt was stirred at room temperature overnight
  2. customThe mixture was partitioned between DCM and water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give a crude oil product, which
  7. customwas used without purification

출처 및 근거

ORD 기록
ord-e134149354544190ab9bd43f7d75f26d
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359359B2

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