4-(Aminomethyl)piperidine → 4-(2,3,5,6-Tetrachloropyridin-4-ylaminomethyl)pyridine

HRID 1957522ノート

反応式

HRID 1957522 の反応式
[N+:1]([C:4]1[C:9]([Cl:10])=[C:8]([Cl:11])[N:7]=[C:6]([Cl:12])[C:5]=1[Cl:13])([O-])=O.N[CH2:15][CH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>O1CCOCC1>[Cl:11][C:8]1[C:9]([Cl:10])=[C:4]([NH:1][CH2:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[C:5]([Cl:13])=[C:6]([Cl:12])[N:7]=1

参加物

4

反応物 2

HCID 235274-(Aminomethyl)piperidineHCID 152291672,3,5,6-Tetrachloro-4-nitropyridine

生成物 1

HCID 190680884-(2,3,5,6-Tetrachloropyridin-4-ylaminomethyl)pyridine収率 24.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

1 g 4-nitro-2,3,5,6-tetrachloropyridine, 0.65 g 4-aminomethylpiperidine and 20 ml absolute dioxane were stirred for 1 hour at room temperature. Subsequently the dioxane was removed by distillation, the residue was admixed with water, separated from undissolved material and the aqueous phase was extracted several times with dichloromethane. After drying and evaporating the solvent, the residue can be crystallized from a small amount of diethyl ether. 0.3 g 4-(2,3,5,6-tetrachloropyridin-4-ylaminomethyl)pyridine is obtained as colourless crystals. TLC (mobile solvent: toluene/dioxane/water 90:20:0.2), Rf=0.8.

後処理

  1. customSubsequently the dioxane was removed by distillation
  2. customseparated from undissolved material
  3. extractionthe aqueous phase was extracted several times with dichloromethane
  4. customAfter drying
  5. customevaporating the solvent
  6. customthe residue can be crystallized from a small amount of diethyl ether

出典と根拠

ORDレコード
ord-84fabf165bc542ec84c65cb7c38a9b47
出典データセット
uspto-grants-1998_07
特許番号
US05786371

反応ノート

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