Methylamine → 1-N'-[(6-chloropyridin-3-yl)methyl]-1-N-methyl-2-nitroethene-1,1-diamine

HRID 249508ノート

反応式

HRID 249508 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][C:10](SC)=[CH:11][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1.[CH3:17][NH2:18]>CCO>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]([NH:18][CH3:17])=[CH:11][N+:12]([O-:14])=[O:13])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 855929321-(6-Chloro-3-pyridylmethyl)amino-1-methylthio-2-nitroethylene

生成物 1

HCID 43256191-N'-[(6-chloropyridin-3-yl)methyl]-1-N-methyl-2-nitroethene-1,1-diamine収率 53.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In 100 ml of EtOH was dissolved 1.2 g (4.6×10-3 mole) of 1-(6-chloro-3-pyridylmethyl)amino-1-methylthio-2-nitroethylene and on reflux, a solution of 0.84 g of 40% aqueous methylamine in 30 ml EtOH was added dropwise over 1 hour. After cooling, the reaction mixture was concentrated under reduced pressure to about 50 ml and the resulting crystals were collected by filtration and dried to give 0.6 g of the title compound as pale yellow needles.

後処理

  1. temperatureon reflux
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated under reduced pressure to about 50 ml
  4. filtrationthe resulting crystals were collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-659fbe34b189419289ea8e87ff3e23ac
出典データセット
uspto-grants-1993_05
特許番号
US05214152

反応ノート

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