1-Methylthio-1-methylamino-2-nitroethylene → HCID 70019858、化合物

HRID 1358698ノート

反応式

HRID 1358698 の反応式
[CH3:1][NH:2][C:3](SC)=[CH:4][N+:5]([O-:7])=[O:6].[CH3:10][N:11]([C:13]1[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:23])([F:22])[F:21])=[CH:15][N:14]=1)[NH2:12]>O1CCOCC1>[CH3:1][NH:2][C:3]([NH:12][N:11]([CH3:10])[C:13]1[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:22])([F:21])[F:23])=[CH:15][N:14]=1)=[CH:4][N+:5]([O-:7])=[O:6]

参加物

4

反応物 2

HCID 1235491-Methylthio-1-methylamino-2-nitroethyleneHCID 27367033-Chloro-2-(1-methylhydrazinyl)-5-(trifluoromethyl)pyridine

生成物 1

HCID 70019858HCID 70019858、化合物収率 33.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

500 mg of N-methyl-1-methylthio-2-nitroetheneamine, 770 mg of 1-methyl-1-(3-chloro-5-trifluoromethyl-2-pyridyl)hydrazine and 7 ml of 1,4-dioxane were stirred for about 4 hours under heating and refluxing and then cooled to room temperature, and the solvent was distilled off under reduced pressure. The concentrated residue was purified by silica gel column chromatography to obtain 370 mg of N-methyl-1-(2-methyl-2-(3-chloro-5-trifluoromethyl-2-pyridyl)hydrazino)-2-nitroetheneamine (Compound No. 35) having a melting point of from 159 to 160° C. (decomposed).

後処理

  1. temperatureunder heating
  2. temperaturerefluxing
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe concentrated residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-a1ccacc6ed2e4e09bf4f0b505d4e64cc
出典データセット
uspto-grants-2003_07
特許番号
US06596863B2

反応ノート

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