Methyl iodide → 3-(4-Nitro-phenyl)-acrylic acid methyl ester

HRID 704398

반응식

HRID 704398 반응식
[N+:1]([C:4]1[CH:14]=[CH:13][C:7]([CH:8]=[CH:9][C:10]([OH:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].CI.[C:17](=O)([O-])[O-].[K+].[K+]>CC(C)=O>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH:8]=[CH:9][C:10]([O:12][CH3:17])=[O:11])=[CH:13][CH:14]=1)([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 701562-Propenoic acid, 3-(4-nitrophenyl)-

생성물 1

HCID 2196853-(4-Nitro-phenyl)-acrylic acid methyl ester수율 53%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 5.80 g of p-nitrocinnamic acid, 10.4 g of methyl iodide, 10.4 g of anhydrous potassium carbonate and 200 ml of acetone was stirred at room temperature for 2 days. The resultant precipitate was filtered off, the filtrate was concentrated under reduced pressure and, after addition of water, the residue was extracted with ethyl acetate. The organic layer was washed with saturated solution of sodium hydrogen carbonate and saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 3.30 g of methyl 4-nitrocinnamate.

후처리

  1. filtrationThe resultant precipitate was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionafter addition of water
  4. extractionthe residue was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated solution of sodium hydrogen carbonate and saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0bb826eff5c84b3cabe4eb8ffa8d9c7c
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987132

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