Ammonium nitrate → 3,5-diethylpyridine

HRID 851321노트

반응식

HRID 851321 반응식
[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]

참가 물질

6

반응물 2

HCID 22985Ammonium nitrateHCID 20502186HCID 20502186, 화합물

생성물 1

HCID 122014443,5-diethylpyridine수율 64%

시약·촉매·용매 3

HCID 176Acetic Acid용매2회HCID 944Nitric Acid용매HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-441e026812164be19f60c3abb0caaaee
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04384120

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