Hydrochloric Acid → 5-(3,4-Dimethoxy-5-chlorophenyl)-2,4-pentadienoic acid

HRID 1088855ノート

反応式

HRID 1088855 の反応式
[CH3:1][O:2][C:3]1[C:4]([O:12][CH3:13])=[C:5](C=C(Cl)C=1)C=O.[C:14]([O:19]CC)(=[O:18])/[CH:15]=[CH:16]/[CH3:17].[CH3:22][C:23]([CH3:26])([O-])[CH3:24].[K+].[ClH:28]>CN1CCCC1=O>[CH3:1][O:2][C:3]1[CH:22]=[C:23]([CH:26]=[CH:17][CH:16]=[CH:15][C:14]([OH:19])=[O:18])[CH:24]=[C:5]([Cl:28])[C:4]=1[O:12][CH3:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 429065Ethyl trans-crotonateHCID 41722755-Chloro-2,3-dimethoxybenzaldehydeHCID 23665647Potassium tert-butoxide

生成物 1

HCID 542197795-(3,4-Dimethoxy-5-chlorophenyl)-2,4-pentadienoic acid

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

To a solution containing 10.0 g of dimethoxy-5-chlorobenzaldehyde and 8.3 ml of ethyl crotonate in 65 ml of N-methylpyrrolidone 6.7 g of potassium tert.-butoxide was added with stirring. The solution was stirred for 0.5 h more at 20° C. and the solution was poured then to a mixture of ice and hydrochloric acid and extracted with ether. The ether extract was washed with water and extracted then with NaHCO3 -solution. The aqueous phase was acidified with hydrochloric acid and the semisolid product was separated and washed with water. Yield 7.3 g (55%).

後処理

  1. additionwas added
  2. stirringThe solution was stirred for 0.5 h more at 20° C.
  3. additionthe solution was poured
  4. extractionextracted with ether
  5. extractionThe ether extract
  6. washwas washed with water
  7. extractionextracted
  8. customthe semisolid product was separated
  9. washwashed with water

出典と根拠

ORDレコード
ord-e6263416a201468591420a2156fdb527
出典データセット
uspto-grants-1990_10
特許番号
US04963590

反応ノート

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