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Acetic Anhydride → (4-Ethoxy-3,5-dimethyl-2-pyridyl)methyl acetate

HRID 979861
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HRID 979861 반응식
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[CH2:8]([O:10][C:11]1[C:16](C)=[CH:15][N+:14]([O-])=[C:13](C)[C:12]=1[CH3:20])[CH3:9]>C(Cl)(Cl)Cl>[C:5]([O:4][CH2:1][C:2]1[C:16]([CH3:15])=[C:11]([O:10][CH2:8][CH3:9])[C:12]([CH3:20])=[CH:13][N:14]=1)(=[O:7])[CH3:6]
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참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 221514664-Ethoxy-2,3,5-trimethylpyridine 1-oxide

생성물 1

HCID 22151469(4-Ethoxy-3,5-dimethyl-2-pyridyl)methyl acetate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

75 ml of acetic anhydride were added dropwise at room temperature to a solution of 31.3 g of 4-ethoxy-2,3,5-trimethylpyridine 1-oxide in 100 ml of chloroform. After boiling under reflux for 16 hours the solution was evaporated, the residue was dissolved in 100 ml of toluene and again evaporated. The residue was taken up in 250 ml of ethyl acetate, whereupon it was extracted three times with 100 ml of saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and evaporated in vacuo. The product was chromatographed on 170 g of silica gel with ether. There was obtained (4-ethoxy-3,5-dimethyl-2-pyridyl)methyl acetate in the form of an oil.

후처리

  1. temperatureunder reflux for 16 hours the solution
  2. customwas evaporated
  3. dissolutionthe residue was dissolved in 100 ml of toluene
  4. customagain evaporated
  5. extractionwas extracted three times with 100 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 170 g of silica gel with ether

출처 및 근거

ORD 기록
ord-1ffbaa5db98e4272b0babdf4cddbeaf1
출처 데이터셋
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04634710

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