Hydrochloric Acid → 3-(1,5-Dimethyl-1H-pyrazol-4-yl)-2-propenoic acid

HRID 30680ノート

反応式

HRID 30680 の反応式
[CH3:1][N:2]1[C:6]([CH3:7])=[C:5](/[CH:8]=[CH:9]/[C:10]([O:12]CC)=[O:11])[CH:4]=[N:3]1.[OH-].[Na+].Cl>CO>[CH3:1][N:2]1[C:6]([CH3:7])=[C:5](/[CH:8]=[CH:9]/[C:10]([OH:12])=[O:11])[CH:4]=[N:3]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 83766845ethyl (2E)-3-(1,5-dimethyl-1H-pyrazol-4-yl)acrylate

生成物 1

HCID 53740613-(1,5-Dimethyl-1H-pyrazol-4-yl)-2-propenoic acid収率 87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

To a mixture of ethyl (2E)-3-(1,5-dimethyl-1H-pyrazol-4-yl)acrylate (380 mg) and methanol (20 ml) was added a 2N aqueous sodium hydroxide solution (2.0 ml), and the mixture was stirred at 60° C. for 14 hrs. 1N Hydrochloric acid was poured into the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated. Recrystallization of the residue from ethyl acetate-hexane gave (2E)-3-(1,5-dimethyl-1H-pyrazol-4-yl)acrylic acid (283 mg, 87%) as colorless prism crystals. melting point: 217-219° C.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customRecrystallization of the residue from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-91129ba6995c4c1d98c84d0f73224267
出典データセット
uspto-grants-2008_09
特許番号
US07423159B2

反応ノート

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