Methyl 3-(dimethylamino)acrylate → Methyl 4-(2,3-dichlorophenyl)-1H-pyrrole-3-carboxylate

HRID 247628

반응식

HRID 247628 반응식
Cl.[Cl:2][C:3]1[C:12]([Cl:13])=[CH:11][CH:10]=[CH:9][C:4]=1[C:5](=O)[CH2:6][NH2:7].CN(C)[CH:16]=[CH:17][C:18]([O:20][CH3:21])=[O:19].CC[O-].[Na+]>C(O)C>[C:18]([C:17]1[C:5]([C:4]2[CH:9]=[CH:10][CH:11]=[C:12]([Cl:13])[C:3]=2[Cl:2])=[CH:6][NH:7][CH:16]=1)([O:20][CH3:21])=[O:19]

참가 물질

5

반응물 3

HCID 566587Methyl 3-(dimethylamino)acrylateHCID 2723922Sodium ethoxideHCID 22151845Ethanone, 2-amino-1-(2,3-dichlorophenyl)-, hydrochloride

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

10.7 g of 2,3-dichlorophenacylamine hydrochloride and 6 g of methyl 3-dimethylaminoacrylate are heated for 2 hours under reflux in 120 ml of ethanol. Then a solution of 4 g of sodium ethylate in 40 ml of ethanol is added dropwise and the reaction mixture is heated for another hour under reflux. The reaction mixture is then concentrated by evaporation and the oily residue is purified by column chromatography (silica gel; elution with a 3:1 mixture of toluene/ethyl acetate. Melting point: 205°-206° C.

후처리

  1. temperaturethe reaction mixture is heated for another hour
  2. temperatureunder reflux
  3. concentrationThe reaction mixture is then concentrated by evaporation
  4. customthe oily residue is purified by column chromatography (silica gel
  5. washelution
  6. additionwith a 3:1 mixture of toluene/ethyl acetate

출처 및 근거

ORD 기록
ord-750983bedfe549e1acd00975d504a47a
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04709053

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