Lithium Hydroxide → 1-Methyl-5-(1H-pyrrol-1-yl)-1H-pyrazole-4-carboxylic acid

HRID 12819ノート

反応式

HRID 12819 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH3:16])[C:10]=1[N:11]1[CH:15]=[CH:14][CH:13]=[CH:12]1)=[O:5])C.[Li+].[OH-]>CO.O>[CH3:16][N:9]1[C:10]([N:11]2[CH:15]=[CH:14][CH:13]=[CH:12]2)=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 2777484Ethyl 1-methyl-5-(1H-pyrrol-1-yl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 155002461-Methyl-5-(1H-pyrrol-1-yl)-1H-pyrazole-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carboxylic acid ethyl ester (20 g, 91.2 mmol; available from Butt Park Ltd., Camelford, Cornwall, UK) in methanol (100 mL) and water (100 mL) was added LiOH (2.4 g, 100 mmol). The reaction mixture was stirred at reflux for 4 hours and then concentrated under reduced pressure to remove the methanol. The residue was diluted with water, acidified to pH 2 with concentrated HCl (9 mL), and extracted with ethyl acetate. The combined extracts were evaporated in vacuo to give 1-methyl-5-pyrrol-1-yl-1H-pyrazole-4-carboxylic acid which was used without further purification.

後処理

  1. temperatureat reflux for 4 hours
  2. concentrationconcentrated under reduced pressure
  3. customto remove the methanol
  4. additionThe residue was diluted with water
  5. extractionextracted with ethyl acetate
  6. customThe combined extracts were evaporated in vacuo

出典と根拠

ORDレコード
ord-38ba975219f44ca7a80bbe24efdc91b0
出典データセット
uspto-grants-2010_06
特許番号
US07728029B2

反応ノート

読み込み中…