Methylene bis(chlorosulfate) → Methanediol, 1,1-dimethanesulfonate

HRID 1021004

反応式

HRID 1021004 の反応式
[S:1](Cl)([O:4][CH2:5]OS(Cl)(=O)=O)(=[O:3])=[O:2].[NH+]1C=CC=C[CH:13]=1.[CH3:18][S:19]([O-:22])(=[O:21])=[O:20]>C(=O)(OC)OC>[CH3:18][S:19]([O:22][CH2:5][O:4][S:1]([CH3:13])(=[O:3])=[O:2])(=[O:21])=[O:20]

参加物

4

反応物 2

HCID 9837734Methylene bis(chlorosulfate)HCID 86654378HCID 86654378、化合物

生成物 1

HCID 9083Methanediol, 1,1-dimethanesulfonate

試薬・触媒・溶媒 1

HCID 12021Dimethyl Carbonate溶媒

実験手順

In dimethyl carbonate (10 mL), methylene bis(chlorosulfate) [CISO2OCH2OSO2Cl] (1.5 g, 6.1 mmol) synthesized on the basis of the method described in U.S. Pat. No. 4,649,209 was reacted with methanesulfonic acid pyridinium salt (2.1 g, 12.0 mmol) under agitation at 55° C. for 3 hours. After the reaction was completed, precipitated chlorosulfonic acid pyridinium salt was separated through filtration, and concentration was performed under reduced pressure, so as to obtain a light brown solid. An adsorption treatment with activated carbon was performed and, thereafter, refining was performed through recrystallization, so as to obtain a desired product, methylene bis(methanesulfonate), at a yield of 48% (0.6 g, 2.9 mmol). The measurement result of 1H NMR is as described below.

後処理

  1. customprecipitated chlorosulfonic acid pyridinium salt
  2. customwas separated through filtration, and concentration
  3. customso as to obtain a light brown solid
  4. customrefining was performed through recrystallization

出典と根拠

ORDレコード
ord-c8ae25f18b394456900ba94ecbd97595
出典データセット
uspto-grants-2014_05
特許番号
US08716513B2

関連ノート

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