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

HRID 983045ノート

反応式

HRID 983045 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1ad93bea9e8d48e8afd14a00e43dc147
出典データセット
uspto-grants-2005_03
特許番号
US06861418B2

反応ノート

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