Hydrochloric Acid → 4-(2,3-Dichlorophenyl)-1H-pyrrole-3-carboxylic acid

HRID 247629노트

반응식

HRID 247629 반응식
[C:1]([C:5]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([Cl:16])[C:11]=2[Cl:17])=[CH:8][NH:7][CH:6]=1)([O:3]C)=[O:2].Cl>CO>[Cl:17][C:11]1[C:12]([Cl:16])=[CH:13][CH:14]=[CH:15][C:10]=1[C:9]1[C:5]([C:1]([OH:3])=[O:2])=[CH:6][NH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 15087831Methyl 4-(2,3-dichlorophenyl)-1H-pyrrole-3-carboxylate

생성물 1

HCID 152390934-(2,3-Dichlorophenyl)-1H-pyrrole-3-carboxylic acid

시약·촉매·용매 1

HCID 887Methanol용매

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온도
70 °C

실험 절차

3.2 g of the 3-carboxethoxy-4-(2,3-dichlorophenyl)pyrrole obtained in (a) and 40 ml of a 1:1 mixture of methanol and 5N HCl are stirred for hours at 70° C. After it has cooled to room temperature, the reaction mixture is poured onto ice and extracted with ethyl acetate. The ester phase is in turn extracted with 10% sodium hydroxide solution. The aqueous extract is washed twice with ethyl acetate, acidified with hydrochloric acid and extracted with ethyl acetate. The organic phase is washed with water, dried over magnesium sulfate and filtered. The filtrate is concentrated by evaporation and the resultant 4-(2,3-dichlorphenyl)pyrrole-3-carboxylic acid melts at 180°-182° C.

후처리

  1. temperatureAfter it has cooled to room temperature
  2. additionthe reaction mixture is poured onto ice
  3. extractionextracted with ethyl acetate
  4. extractionextracted with 10% sodium hydroxide solution
  5. extractionThe aqueous extract
  6. washis washed twice with ethyl acetate
  7. extractionextracted with ethyl acetate
  8. washThe organic phase is washed with water
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. concentrationThe filtrate is concentrated by evaporation

출처 및 근거

ORD 기록
ord-3593be100b004506a1fca647011df3b3
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04709053

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