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(2,6-Dichloropyridin-3-YL)methanamine → 1-(2,6-Dichloro-3-pyridylmethyl)amino-1-methylamino-2-nitroethylene

HRID 249514
ノート
印刷プレビュー

反応式

HRID 249514 の反応式
[Cl:1][C:2]1[C:7]([CH2:8][NH2:9])=[CH:6][CH:5]=[C:4]([Cl:10])[N:3]=1.[CH3:11][NH:12][CH:13](SC)[CH2:14][N+:15]([O-:17])=[O:16]>CCO>[Cl:1][C:2]1[C:7]([CH2:8][NH:9][C:13]([NH:12][CH3:11])=[CH:14][N+:15]([O-:17])=[O:16])=[CH:6][CH:5]=[C:4]([Cl:10])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 15477284(2,6-Dichloropyridin-3-YL)methanamineHCID 15788612N-Methyl-1-(methylsulfanyl)-2-nitroethan-1-amine

生成物 1

HCID 598966091-(2,6-Dichloro-3-pyridylmethyl)amino-1-methylamino-2-nitroethylene収率 27.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1.2 g (0.007 mole) of (2,6dichloro-3-pyridylmethyl)amine and 1 g (0.007 mole) of 1-methylamino-1-methylthio-2-nitroethane was refluxed in 50 ml of EtOH for 6 hours. After cooling, the reaction mixture was concentrated and the resulting crystals were collected by filtration, washed with CH2Cl2 and a small amount of EtOH in that order and dried. The procedure gave 0.53 g of the title compound as a white powder.

後処理

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture was concentrated
  3. filtrationthe resulting crystals were collected by filtration
  4. washwashed with CH2Cl2
  5. dry with materiala small amount of EtOH in that order and dried

出典と根拠

ORDレコード
ord-a8e6b8a12d474ac785b99ef3e44d02a6
出典データセット
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05214152

反応ノート

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