1-Methylthio-1-methylamino-2-nitroethylene → HCID 70019858, 화합물

HRID 1280393노트

반응식

HRID 1280393 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 70019858HCID 70019858, 화합물수율 33.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6746119f033842d3b84ae240032f3406
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06451792B1

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