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

HRID 12819노트

반응식

HRID 12819 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-38ba975219f44ca7a80bbe24efdc91b0
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728029B2

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