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

HRID 333041노트

반응식

HRID 333041 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eb25510adafd499e8edcda0bb0a3d1ed
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877953B2

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