Trimethylamine → N,N-dimethyl-5-nitropyridin-2-amine

HRID 865668

反応式

HRID 865668 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[CH3:11][N:12](C)[CH3:13]>CCO>[CH3:11][N:12]([CH3:13])[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 1146TrimethylamineHCID 783082-Chloro-5-nitropyridine

生成物 1

HCID 75707N,N-dimethyl-5-nitropyridin-2-amine収率 89.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

A mechanically stirred mixture of 2-chloro-5-nitropyridine (56.25 g, 0.355 mol) and absolute EtOH (960 ml), under nitrogen was treated, during 15 minutes with 25% aqueous trimethylamine (217 g). The mixture warmed to 40° C. and a thick yellow precipitate formed; it was warmed to 80° C. during 1 hour, cooled to ambient temperature and filtered. The solid was washed with cold 20% H2O-EtOH and dried to give 53.2 g of the titled product, m.p. 151°-152° C.

後処理

  1. customa thick yellow precipitate formed
  2. temperatureit was warmed to 80° C. during 1 hour
  3. temperaturecooled to ambient temperature
  4. filtrationfiltered
  5. washThe solid was washed with cold 20% H2O-EtOH
  6. customdried

出典と根拠

ORDレコード
ord-a42ee2f1e2da43618bd597d4a0e3c400
出典データセット
uspto-grants-1996_10
特許番号
US05567722

関連ノート

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