Potassium Hydroxide → 5-Formyl-4-methyl-1H-pyrrole-3-carboxylic acid

HRID 983045

반응식

HRID 983045 반응식
[OH-].[K+].C([O:5][C:6]([C:8]1[C:12]([CH3:13])=[C:11]([CH:14]=[O:15])[NH:10][CH:9]=1)=[O:7])C>O.CCO>[CH:14]([C:11]1[NH:10][CH:9]=[C:8]([C:6]([OH:7])=[O:5])[C:12]=1[CH3:13])=[O:15]

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 236067Ethyl 5-formyl-4-methyl-1h-pyrrole-3-carboxylate

생성물 1

HCID 221354535-Formyl-4-methyl-1H-pyrrole-3-carboxylic acid수율 87.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

KOH (5 g, 2 eq) was added to a suspension of 5-formyl-4-methyl-1H-pyrrole-3-carboxylic acid ethyl ester (8.13 g, 44.8 mmol) in water (100 mL) and EtOH (50 mL) with stirring. The mixture was heated to reflux for 2.5 hr, cooled to rt, concentrated to about ⅔ volume, diluted with water (300 mL) and acidified to pH=3 using 1N HCl. The white solid was collected by filtration and dried to afford 6 g (87%) of 5-formyl-4-methyl-1H-pyrrole-3-carboxylic acid as a tan solid.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 2.5 hr
  3. concentrationconcentrated to about ⅔ volume
  4. additiondiluted with water (300 mL)
  5. filtrationThe white solid was collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-1ad93bea9e8d48e8afd14a00e43dc147
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06861418B2

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