Potassium Hydroxide → (E)-4-(Diethoxyphosphoryl)but-2-enoic acid

HRID 333041ノート

反応式

HRID 333041 の反応式
CC[O:3][C:4](/[CH:6]=[CH:7]/[CH2:8][P:9]([O:14][CH2:15][CH3:16])([O:11][CH2:12][CH3:13])=[O:10])=[O:5].[OH-].[K+]>O>[CH2:15]([O:14][P:9]([CH2:8]/[CH:7]=[CH:6]/[C:4]([OH:5])=[O:3])([O:11][CH2:12][CH3:13])=[O:10])[CH3:16]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 5365783Triethyl 4-phosphonocrotonate, mixture of isomers

生成物 1

HCID 6285301(E)-4-(Diethoxyphosphoryl)but-2-enoic acid収率 89.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

To a solution of triethyl 4-phosphonocrotonate (5.53 g) in water (36 mL) was added a solution of potassium hydroxide (1.69 g) in water (36 mL) at room temperature, and the reaction solution was stirred for 3 hours. The resulting reaction solution was washed with dichloromethane, and the water layer was acidified to pH2 with concentrated hydrochloric acid and extracted with dichloromethane (550 mL). The combined organic layer was dried over anhydrous magnesium sulfate and concentrated to dryness under reduced pressure to give 4.41 g of 4-diethylphosphonocrotonic acid as a colorless solid.

後処理

  1. customThe resulting reaction solution
  2. washwas washed with dichloromethane
  3. extractionextracted with dichloromethane (550 mL)
  4. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-eb25510adafd499e8edcda0bb0a3d1ed
出典データセット
uspto-grants-2014_11
特許番号
US08877953B2

反応ノート

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