Methyl fluorosulfate → 2-Methyl-3-methoxy-1,2,5-thiadiazolium Fluorosulfonate

HRID 1704639노트

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HRID 1704639 반응식
[CH3:1][N:2]1[C:6](=[O:7])[CH:5]=[N:4][S:3]1.[F:8][S:9]([O:12][CH3:13])(=[O:11])=[O:10]>C(Cl)Cl>[F:8][S:9]([O-:12])(=[O:11])=[O:10].[CH3:1][N+:2]1[S:3][N:4]=[CH:5][C:6]=1[O:7][CH3:13]

참가 물질

4

반응물 2

HCID 9870Methyl fluorosulfate2회HCID 124954582-Methyl-1,2,5-thiadiazole-3-one

생성물 1

HCID 124955042-Methyl-3-methoxy-1,2,5-thiadiazolium Fluorosulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Methyl-1,2,5-thiadiazole-3-one (11.6 g., 0.1 mole) was dissolved in dry methylene chloride (100 ml.) and under a nitrogen atmosphere was added methyl fluorosulfonate (8.2 ml., 0.1 mole) and the reaction mixture was stirred at room temperature for 1 hour. Further, methyl fluorosulfonate (0.1 ml.) was added and the reaction continued at reflux for one further hour. The reaction was cooled, the precipitate separated by filtration and washed with several portions of cold methylene chloride. Yield 13 g. The compound was stored in a dry atmosphere, m.p., 138°-139° C.

후처리

  1. temperatureat reflux for one further hour
  2. temperatureThe reaction was cooled
  3. customthe precipitate separated by filtration
  4. washwashed with several portions of cold methylene chloride
  5. customwas stored in a dry atmosphere, m.p., 138°-139° C.

출처 및 근거

ORD 기록
ord-b005a1a1b05a492a9c356c16f9c9eb0a
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04127584

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