2-Chloro-5-nitropyridine → HCID 4418042、化合物

HRID 1030997ノート

反応式

HRID 1030997 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>C(NCC)C.C(Cl)Cl>[CH2:2]([N:3]([CH2:4][CH3:5])[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1)[CH3:7]

参加物

4

反応物 1

HCID 783082-Chloro-5-nitropyridine

生成物 1

HCID 4418042HCID 4418042、化合物収率 195.5%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8021Diethylamine溶媒

実験手順

A stirred mixture of 27.6 g (0.174 mole) of 2-chloro-5-nitropyridine in 500 ml of diethylamine was heated at reflux for two days. The excess diethylamine was removed by distillation under reduced pressure, leaving a residue. This residue was dissolved in methylene chloride, and the organic solution was washed with an aqueous, 10% sodium hydroxide solution. The washed organic phase was dried over anhydrous magnesium sulfate and was filtered. The filtrate was evaporated under reduced pressure to yield 33.2 g of 2-diethylamino-5-nitropyridine as a solid. The nmr spectrum was consistent with the proposed structure.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for two days
  3. customThe excess diethylamine was removed by distillation under reduced pressure
  4. customleaving a residue
  5. washthe organic solution was washed with an aqueous, 10% sodium hydroxide solution
  6. dry with materialThe washed organic phase was dried over anhydrous magnesium sulfate
  7. filtrationwas filtered
  8. customThe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ce5c4d0c44d6447eb50a8d7463a72ce8
出典データセット
uspto-grants-1992_04
特許番号
US05108486

反応ノート

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