Lithium Hydroxide → 5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid

HRID 12921ノート

反応式

HRID 12921 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH:12]2[CH2:15][CH2:14][CH2:13]2)[C:10]=1[Cl:11])=[O:5])C.[Li+].[OH-]>CO.O>[Cl:11][C:10]1[N:9]([CH:12]2[CH2:13][CH2:14][CH2:15]2)[N:8]=[CH:7][C:6]=1[C:4]([OH:5])=[O:3]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 58972820HCID 58972820、化合物

生成物 1

HCID 589728585-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid収率 94%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid ethyl ester (182 mg, 0.79 mmol) in methanol (8 mL) and water (8 mL) was added LiOH (23 mg, 0.96 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 and extracted with ethyl acetate. The organic layer was evaporated in vacuo to give 5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid (148 mg, 94%) 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 organic layer was evaporated in vacuo

出典と根拠

ORDレコード
ord-dd3268c8f97946cc86e36fdf228ddcd2
出典データセット
uspto-grants-2010_06
特許番号
US07728029B2

反応ノート

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