Methylamine → 1-Methylamino-1-(3-pyridylmethyl)amino-2-nitroethylene

HRID 1682219ノート

反応式

HRID 1682219 の反応式
CS[C:3]([NH:8][CH2:9][C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=[CH:4][N+:5]([O-:7])=[O:6].[CH3:16][NH2:17]>CCO>[CH3:16][NH:17][C:3]([NH:8][CH2:9][C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=[CH:4][N+:5]([O-:7])=[O:6]

参加物

4

反応物 2

HCID 6329MethylamineHCID 70155832HCID 70155832、化合物

生成物 1

HCID 701581981-Methylamino-1-(3-pyridylmethyl)amino-2-nitroethylene収率 76.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In 50 ml of EtOH was dissolved 2.3 g (0.01 mole) of 1-methylthio-1-(3-pyridylmethyl)amino-2-nitroethylene with heating and, then, a solution of 1.2 g (0.015 mole) of 40% aqueous methylamine in 10 ml of EtOH was added dropwise over a period of 30 minutes while refluxing. The mixture was further refluxed for 2 hours, after which it was concentrated. The crystals were collected by filtration and recrystallized from acetonitrile to give 1.6 g of the title compound as white prisms.

後処理

  1. temperaturewith heating
  2. temperaturewhile refluxing
  3. temperatureThe mixture was further refluxed for 2 hours
  4. concentrationafter which it was concentrated
  5. filtrationThe crystals were collected by filtration
  6. customrecrystallized from acetonitrile

出典と根拠

ORDレコード
ord-7fd1b3b3d44642da82df2c39943977cb
出典データセット
uspto-grants-1992_12
特許番号
US05175301

反応ノート

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