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

HRID 704398

反応式

HRID 704398 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0bb826eff5c84b3cabe4eb8ffa8d9c7c
出典データセット
uspto-grants-1991_01
特許番号
US04987132

関連ノート

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