Hydrochloric Acid → (2E)-3-(1-methyl-1H-pyrazol-4-yl)prop-2-enoic acid

HRID 30682

反応式

HRID 30682 の反応式
[CH3:1][N:2]1[CH:6]=[C:5](/[CH:7]=[CH:8]/[C:9]([O:11]CC)=[O:10])[CH:4]=[N:3]1.CO.[OH-].[Na+].Cl>O1CCCC1>[CH3:1][N:2]1[CH:6]=[C:5](/[CH:7]=[CH:8]/[C:9]([OH:11])=[O:10])[CH:4]=[N:3]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 68356132(E)-Ethyl 3-(1-methyl-1H-pyrazol-4-yl)acrylate

生成物 1

HCID 1529858(2E)-3-(1-methyl-1H-pyrazol-4-yl)prop-2-enoic acid収率 83%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

To a mixture of ethyl (2E)-3-(1-methyl-1H-pyrazol-4-yl)acrylate (2.5 g), methanol (20 ml) and tetrahydrofuran (20 ml) was added a 2N aqueous sodium hydroxide solution (13.9 ml) and the mixture was stirred at 60° C. for 3 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 to give (2E)-3-(1-methyl-1H-pyrazol-4-yl)acrylic acid (1.75 g, 83%) as an amorphous form.

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

出典と根拠

ORDレコード
ord-e3995dd47bdf448cb9568a52cff09b20
出典データセット
uspto-grants-2008_09
特許番号
US07423159B2

関連ノート

読み込み中…