N1-(pyridin-4-yl)ethane-1,2-diamine → HCID 14834211、化合物

HRID 476997

反応式

HRID 476997 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([NH:7][CH2:8][CH2:9][NH2:10])=[CH:3][CH:2]=1.[N+:11]([C:14]1[CH:23]=[CH:22][CH:21]=[CH:20][C:15]=1[CH:16]=[CH:17][CH2:18]Cl)([O-:13])=[O:12]>C(O)C>[N+:11]([C:14]1[CH:23]=[CH:22][CH:21]=[CH:20][C:15]=1/[CH:16]=[CH:17]/[CH2:18][NH:10][CH2:9][CH2:8][NH:7][C:4]1[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=1)([O-:13])=[O:12]

参加物

4

反応物 2

HCID 14834209N1-(pyridin-4-yl)ethane-1,2-diamineHCID 544529242-Nitro-cinnamyl chloride

生成物 1

HCID 14834211HCID 14834211、化合物収率 29.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 11 g of N-(4-pyridyl)ethylenediamine and 5.3 g of 2-nitrocinnamyl chloride (trans-form) dissolved in 60 ml of ethanol was stirred at room temperature for 30 minutes and then stirred at 50° C. for 90 minutes. The solvent was distilled off under reduced pressure, and 10% aqueous sodium hydroxide was added to the residue and the mixture was extracted with chloroform. After drying of the extract, chloroform was distilled off and the residue was purified by silica gel column chromatography (solvent: chloroform-methanol-triethylamine=20:1:0.1) to give 2.33 g of (E)-N-(2-nitrocinnamyl)-N'-(4-pyridyl)ethyenediamine as a yellow oily substance.

後処理

  1. stirringstirred at 50° C. for 90 minutes
  2. distillationThe solvent was distilled off under reduced pressure, and 10% aqueous sodium hydroxide
  3. additionwas added to the residue
  4. extractionthe mixture was extracted with chloroform
  5. dry with materialAfter drying of the extract, chloroform
  6. distillationwas distilled off
  7. customthe residue was purified by silica gel column chromatography (solvent: chloroform-methanol-triethylamine=20:1:0.1)

出典と根拠

ORDレコード
ord-53b279c9fa014745a936af0648eec4dd
出典データセット
uspto-grants-1989_12
特許番号
US04886817

関連ノート

読み込み中…