Ethanol → Ethyl 3-(3-bromophenyl)acrylate

HRID 441559ノート

反応式

HRID 441559 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7]([OH:9])=[O:8].S(=O)(=O)(O)O.[CH2:18](O)[CH3:19]>>[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)/[CH:5]=[CH:6]/[C:7]([O:9][CH2:18][CH3:19])=[O:8]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 776461m-Bromocinnamic acid

生成物 1

HCID 5369361Ethyl 3-(3-bromophenyl)acrylate

実験手順

Trans m-bromocinnamic acid (14.8 g), ethanol (173 ml) and concentrated sulfuric acid (0.4 ml) were combined and heated at reflux for 15 hours. About 150 ml of the ethanol was distilled off, and the remaining solution was poured into ice/water (140 ml). The cold mixture was made strongly alkaline with 40% sodium hydroxide and extracted with methylene chloride (4 × 60 ml). The combined methylene chloride extract was dried over anhydrous potassium carbonate. The potassium carbonate was removed by filtration and the solvent stripped off under reduced pressure. Trans ethyl 3-bromocinnamate, was obtained as a partially solidified oil. (IR spectrum was consistent with this compound).

後処理

  1. temperatureheated
  2. temperatureat reflux for 15 hours
  3. distillationAbout 150 ml of the ethanol was distilled off
  4. additionthe remaining solution was poured into ice/water (140 ml)
  5. extractionextracted with methylene chloride (4 × 60 ml)
  6. extractionThe combined methylene chloride extract
  7. dry with materialwas dried over anhydrous potassium carbonate
  8. customThe potassium carbonate was removed by filtration

出典と根拠

ORDレコード
ord-422d768d7240489ab750774473af4564
出典データセット
uspto-grants-1977_08
特許番号
US04041071

反応ノート

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