Water → 4-(3-dimethylaminopropyl)-5-formyl-2-methyl-1H-pyrrole-3-carboxylic acid

HRID 1860875

反応式

HRID 1860875 の反応式
C([O:3][C:4]([C:6]1[C:10]([CH2:11][CH2:12][CH2:13][N:14]([CH3:16])[CH3:15])=[C:9]([CH:17]=[O:18])[NH:8][C:7]=1[CH3:19])=[O:5])C.[OH-].[Na+].O>CO.CCOC(C)=O>[CH3:16][N:14]([CH3:15])[CH2:13][CH2:12][CH2:11][C:10]1[C:6]([C:4]([OH:5])=[O:3])=[C:7]([CH3:19])[NH:8][C:9]=1[CH:17]=[O:18]

参加物

6

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 542399104-(3-dimethylaminopropyl)-5-formyl-2-methyl-1H-pyrrole-3-carboxylic acid ethyl ester

生成物 1

HCID 225710744-(3-dimethylaminopropyl)-5-formyl-2-methyl-1H-pyrrole-3-carboxylic acid収率 94%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4-(3-dimethylaminopropyl)-5-formyl-2-methyl-1H-pyrrole-3-carboxylic acid ethyl ester (300 mg, 1.13 mmol) and sodium hydroxide in MeOH (4 mL)/water (2 mL) was stirred at 80° C. for 19 hr. The reaction was then diluted with EtOAc. The aqueous layer was separated, neutralized and concentrated. The residue was dissolved in MeOH, filtered and the filtrate was concentrated to give 251 mg (94%) of 4-(3-dimethylaminopropyl)-5-formyl-2-methyl-1H-pyrrole-3-carboxylic acid.

後処理

  1. customThe aqueous layer was separated
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in MeOH
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-cbebf8a6be8546749247328f611865ed
出典データセット
uspto-grants-2003_03
特許番号
US06531502B1

関連ノート

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