Dimethyl Carbonate → HCID 86665804、化合物

HRID 1021006

反応式

HRID 1021006 の反応式
[S:1](Cl)([O:4][CH2:5][O:6][S:7](Cl)(=[O:9])=[O:8])(=[O:3])=[O:2].[NH+]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[CH3:18][O:19][C:20]1[CH:25]=[CH:24][C:23](S([O-])(=O)=O)=[CH:22][CH:21]=1.[C:30](=O)(OC)[O:31][CH3:32]>>[CH3:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([S:1]([O:4][CH2:5][O:6][S:7]([C:15]2[CH:16]=[CH:17][C:30]([O:31][CH3:32])=[CH:13][CH:14]=2)(=[O:9])=[O:8])(=[O:3])=[O:2])=[CH:22][CH:21]=1

参加物

4

反応物 3

HCID 12021Dimethyl CarbonateHCID 9837734Methylene bis(chlorosulfate)HCID 89599766HCID 89599766、化合物

生成物 1

HCID 86665804HCID 86665804、化合物

実験手順

In dimethyl carbonate (30 mL), methylene bis(chlorosulfate) [CISO2OCH2OSO2Cl] (4.5 g, 13 mmol) was reacted with 4-methoxybenzenesulfonic acid pyridinium salt (7 g, 26 mmol) under agitation at 55° C. for 2 hours. After the reaction was completed, precipitated chlorosulfonic acid pyridinium salt was separated through filtration. Washing with water was performed and, subsequently, concentration was performed under reduced pressure, so as to obtain a pale red transparent oil. Refining was performed through recrystallization, so as to obtain a desired product, methylene bis(4-methoxybenzenesulfonate), at a yield of 32% (1.65 g, 4.2 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
  3. washWashing with water
  4. concentrationsubsequently, concentration
  5. customso as to obtain a pale red transparent oil
  6. customRefining was performed through recrystallization

出典と根拠

ORDレコード
ord-d4701e1f41334bc4b486c049b3469ab2
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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