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

HRID 2200573

反応式

HRID 2200573 の反応式
[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]

参加物

4

反応物 2

HCID 8134Diethylene Glycol Monomethyl EtherHCID 31297Methanesulfonyl chloride

生成物 1

HCID 38156542-(2-Methoxyethoxy)ethyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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]

後処理

  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

出典と根拠

ORDレコード
ord-e134149354544190ab9bd43f7d75f26d
出典データセット
uspto-grants-2016_06
特許番号
US09359359B2

関連ノート

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