Ammonium nitrate → 3,5-diethylpyridine

HRID 851321ノート

反応式

HRID 851321 の反応式
[CH2:1]([CH:3]1[CH2:8][C:7]([CH2:9][CH3:10])=[CH:6]O[CH:4]1OC)[CH3:2].[N+:13]([O-])([O-])=O.[NH4+]>O.C(O)(=O)C.[N+]([O-])(O)=O>[CH2:1]([C:3]1[CH:4]=[N:13][CH:6]=[C:7]([CH2:9][CH3:10])[CH:8]=1)[CH3:2]

参加物

6

反応物 2

HCID 22985Ammonium nitrateHCID 20502186HCID 20502186、化合物

生成物 1

HCID 122014443,5-diethylpyridine収率 64%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒2 回HCID 944Nitric Acid溶媒HCID 962Water溶媒2 回

実験手順

170 parts of 3,5-diethyl-2,3-dihydro-2-methoxy-4H-pyran are dissolved in 25 parts of water, 300 parts of acetic acid and 2 parts of 60 percent strength nitric acid at 22° C. After 15 minutes, a solution of 88 parts of ammonium nitrate in 80 parts of water is added. The resulting solution is run into 800 parts of acetic acid at 110° C. in the course of 20 minutes, whilst stirring. The reaction mixture is left to cool, the acetic acid, water and methanol are distilled off, 200 parts of water are added to the residue and the solution is rendered alkaline with 25 percent strength ammonia solution. The 3,5-diethylpyridine is extracted with ether. Distillation gives 87 parts (64% of theory) of 3,5-diethylpyridine of boiling point 92° C./15 mm Hg.

後処理

  1. waitThe reaction mixture is left
  2. temperatureto cool
  3. distillationthe acetic acid, water and methanol are distilled off
  4. addition200 parts of water are added to the residue
  5. extractionThe 3,5-diethylpyridine is extracted with ether
  6. distillationDistillation

出典と根拠

ORDレコード
ord-441e026812164be19f60c3abb0caaaee
出典データセット
uspto-grants-1983_05
特許番号
US04384120

反応ノート

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