Dimethyl Carbonate → Methylene bis(4-methoxybenzenesulfonate)

HRID 1021006

반응식

HRID 1021006 반응식
[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

참가 물질

4

반응물 3

HCID 12021Dimethyl CarbonateHCID 9837734Methylene bis(chlorosulfate)HCID 89599766HCID 89599766, 화합물

생성물 1

HCID 86665804Methylene bis(4-methoxybenzenesulfonate)

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d4701e1f41334bc4b486c049b3469ab2
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716513B2

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