Sodium Hydroxide → 4-bromo-1,3-dimethyl-1H-pyrazole-5-carboxylic acid

HRID 244666

反応式

HRID 244666 の反応式
[Br:1][C:2]1[C:3]([CH3:13])=[N:4][N:5]([CH3:12])[C:6]=1[C:7]([O:9]CC)=[O:8].[OH-].[Na+]>CO>[Br:1][C:2]1[C:3]([CH3:13])=[N:4][N:5]([CH3:12])[C:6]=1[C:7]([OH:9])=[O:8]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 7022226ethyl 4-bromo-1,3-dimethyl-1H-pyrazole-5-carboxylate

生成物 1

HCID 27798334-bromo-1,3-dimethyl-1H-pyrazole-5-carboxylic acid収率 14.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
20 °C

実験手順

To a solution of ethyl 4-bromo-1,3-dimethyl-1H-pyrazole-5-carboxylate (200 mg) (for example, available from Sinova) in methanol (10 ml) was added 2M sodium hydroxide (5 ml) and the mixture stirred at 20° C. for 18 h. The mixture was concentrated in vacuo and the residue taken up in water (10 ml) and acidified to pH=5 using 2M hydrochloric acid. The mixture was extracted with ethyl acetate (20 ml) dried over sodium sulphate and evaporated to give the title compound (25 mg) as a white solid.

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. extractionThe mixture was extracted with ethyl acetate (20 ml)
  3. dry with materialdried over sodium sulphate
  4. customevaporated

出典と根拠

ORDレコード
ord-892f17811ad04ed5ba0471035bfa38ca
出典データセット
uspto-grants-2014_02
特許番号
US08658635B2

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