But-2-yn-1-amine → HCID 178449099、化合物

HRID 2050354

反応式

HRID 2050354 の反応式
[N+:1]([CH:4]=[C:5](SC)[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2].[CH2:19]([NH2:23])[C:20]#[C:21][CH3:22]>C(#N)C>[N+:1]([CH:4]=[C:5]([NH:23][CH2:19][C:20]#[C:21][CH3:22])[NH:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16])([O-:3])=[O:2]

参加物

4

反応物 2

HCID 12599998But-2-yn-1-amineHCID 178503826HCID 178503826、化合物

生成物 1

HCID 178449099HCID 178449099、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 1-nitro-2-methylthio-2-{2-[(4-methyl-1H-imidazol-5-yl)methylthio]ethylamino}ethylene (2.25 g, 7.8 mmole) and 2-butyn-1-amine (2.16 g, 31.2 mmole) in acetonitrile (35 ml) was stirred under a positive pressure of nitrogen at reflux temperature for 7 hours and at room temperature for 15 hours. The solvent was removed by evaporation under reduced pressure, and the residue placed on silica gel and chromatographed by gradient elution using methylene chloride-methanol. The appropriate fractions yielded 1.93 g (80%) of the title product from acetonitrile. Recrystallization from isopropyl alcohol gave the product with mp 147.5°-151°.

後処理

  1. temperatureat reflux temperature for 7 hours
  2. customThe solvent was removed by evaporation under reduced pressure
  3. customchromatographed by gradient elution

出典と根拠

ORDレコード
ord-7061474c2641419e8d05494a9c4f66df
出典データセット
uspto-grants-1980_04
特許番号
US04200760

関連ノート

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