Acetic Anhydride → (4-Ethoxy-5-methyl-2-pyridyl)methyl acetate

HRID 703182노트

반응식

HRID 703182 반응식
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[CH2:8]([O:10][C:11]1[C:16]([CH3:17])=[CH:15][N+:14]([O-])=C(C)[CH:12]=1)[CH3:9]>C(Cl)(Cl)Cl>[C:5]([O:4][CH2:1][C:2]1[CH:12]=[C:11]([O:10][CH2:8][CH3:9])[C:16]([CH3:17])=[CH:15][N:14]=1)(=[O:7])[CH3:6]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 221514414-Ethoxy-2,5-dimethylpyridine 1-oxide

생성물 1

HCID 22151443(4-Ethoxy-5-methyl-2-pyridyl)methyl acetate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

20 ml of acetic anhydride were added dropwise at room temperature to solutio of 7.8 of 4-ethoxy-2.5-dimethylpyridine 1-oxide in 30 ml of chloroform. After boiling under reflux for 3 hours the solution was evaporated, the residue was dissolved in 50 ml of toluene and again evaporated. The residue was taken up in 50 ml of ethyl acetate, whereupon the solution was extracted three times with 20 ml of saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and evaporated in vacuo. The product was chromatographed on 50 g of silica gel with ether and there was obtained (4-ethoxy-5-methyl-2-pyridyl)methyl acetate in the form of an oil.

후처리

  1. temperatureunder reflux for 3 hours the solution
  2. customwas evaporated
  3. dissolutionthe residue was dissolved in 50 ml of toluene
  4. customagain evaporated
  5. extractionwas extracted three times with 20 ml of saturated sodium bicarbonate solution
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. customevaporated in vacuo
  8. customThe product was chromatographed on 50 g of silica gel with ether

출처 및 근거

ORD 기록
ord-add17029bf6a45eb8d062008a35745a4
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04981861

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