反応 #1379887

ord-99b7da3f0cc541afa3e5dc55ff387482

反応方程式

COc1ccc([N+](=O)[O-])c(Cl)n1
2-chloro-3-nitro-6-methoxypyridine
COCCNCCOC
bis(2-methoxyethyl)amine
COCCN(CCOC)c1nc(OC)ccc1[N+](=O)[O-]
yellow powder
収率 90.6%
COCCN(CCOC)c1nc(OC)ccc1[N+](=O)[O-]
bis(2-methoxyethyl)(6-methoxy-3-nitro-2-pyridyl)amine
収率 90.6%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture is refluxed for 2 hours
  2. 2
    workup.STIRRINGwith stirring
  3. 3
    その他The precipitate formed
  4. 4
    ろ過is filtered off by suction
  5. 5
    その他dried under vacuum to constant weight

実験手順

4 g (0.0212 mol) of the product 2-chloro-3-nitro-6-methoxypyridine, 50 ml of ethanol and 6.32 ml (0.0424 mol) of bis(2-methoxyethyl)amine are placed in a fully equipped round-bottomed flask. The mixture is refluxed for 2 hours with stirring and is then poured onto an ice/water mixture with stirring. The precipitate formed is filtered off by suction and dried under vacuum to constant weight. 5.47 g of yellow powder are obtained, ie a yield of 90.6%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07238211B2uspto-grants-2007_07