Hydrochloric Acid → 1,2-Bis(methylsulfonyl)-1,2-dimethylhydrazine

HRID 2372953

반응식

HRID 2372953 반응식
Cl.Cl.[CH3:3][NH:4][NH:5][CH3:6].[CH3:7][S:8](Cl)(=[O:10])=[O:9].Cl>>[CH3:7][S:8]([N:4]([CH3:3])[N:5]([S:8]([CH3:7])(=[O:10])=[O:9])[CH3:6])(=[O:10])=[O:9]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 93801,2-Dimethylhydrazine dihydrochlorideHCID 31297Methanesulfonyl chloride

생성물 1

HCID 150448651,2-Bis(methylsulfonyl)-1,2-dimethylhydrazine수율 32.4%

실험 절차

1,2-Dimethylhydrazine dihydrochloride (2.6 g, 0.02 mol) was suspended in ice-cold dry pyridine (6 ml) and the mixture was stirred for 10 minutes. Methanesulfonyl chloride (5.0 g, 0.043 mol) was added in portions to this mixture, while maintaining the temperature between 0° and 10° C. After an additional 1 hour of stirring at 0° to 5° C., the reaction mixture was left in a freezer (-10° C.) overnight. The pH of the reaction mixture was adjusted to pH 1 with cold dilute hydrochloric acid. The solid that separated was filtered and recrystallized from ethanol (Norit A) to give 1.4 g (32%) of the title compound: m.p. 168°-169° C.; anal. (C4H12N2O4S2) C,H,N; 1H NMR (CDCl3) δ 3.1 [2s, 12H, 2(CH3SO2NCH3)].

후처리

  1. temperaturewhile maintaining the temperature between 0° and 10° C
  2. stirringAfter an additional 1 hour of stirring at 0° to 5° C.
  3. waitthe reaction mixture was left in a freezer (-10° C.) overnight
  4. customThe solid that separated
  5. filtrationwas filtered
  6. customrecrystallized from ethanol (Norit A)

출처 및 근거

ORD 기록
ord-b26857c00251469d96a2144a92a29e4c
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05101072

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