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

HRID 1704639ノート

反応式

HRID 1704639 の反応式
[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]

参加物

4

反応物 2

HCID 9870Methyl fluorosulfate2 回HCID 124954582-Methyl-1,2,5-thiadiazole-3-one

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-b005a1a1b05a492a9c356c16f9c9eb0a
出典データセット
uspto-grants-1978_11
特許番号
US04127584

反応ノート

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