Hydrochloric Acid → 5-(3,4-Dimethoxy-6-chlorophenyl)-2,4-pentadienoic acid

HRID 1974703노트

반응식

HRID 1974703 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:8]([Cl:13])=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=O.[C:14]([O:19]CC)(=[O:18])/[CH:15]=[CH:16]/[CH3:17].CC(C)([O-])C.[K+].Cl>CN1CCCC1=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[CH:17][CH:16]=[CH:15][C:14]([OH:19])=[O:18])[C:8]([Cl:13])=[CH:9][C:10]=1[O:11][CH3:12]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 2793512-Chloro-4,5-dimethoxybenzaldehydeHCID 429065Ethyl trans-crotonateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 540567045-(3,4-Dimethoxy-6-chlorophenyl)-2,4-pentadienoic acid

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

To a solution containing 10.0 g 3,4 dimethoxy-6-chlorobenzaldehyde and 8 ml of ethyl crotonate in 60 ml of N-methylpyrrolidone 6.0 g of potassium tert.-butoxide was added while stirring. The solution was stirred for 0.5 h more at 20° C. and poured then to a mixture of ice and hydrochloric acid. The solution was extracted with ether. The ether solution was washed with water and extracted with 2.5N NaOH-solution. The aqueous phase was acidified with hydrochloric acid and the semisolid product was separated. Yield 10.8 g (81%).

후처리

  1. additionwas added
  2. stirringThe solution was stirred for 0.5 h more at 20° C.
  3. additionpoured
  4. extractionThe solution was extracted with ether
  5. washThe ether solution was washed with water
  6. extractionextracted with 2.5N NaOH-solution
  7. customthe semisolid product was separated

출처 및 근거

ORD 기록
ord-2988787b40d743d4af778fd30a59ad0a
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05283352

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