Ethyl 3-amino-2-phenylpropyl(diethoxymethyl)phosphinate → 3-Amino-2-phenylpropylphosphonous acid

HRID 622897

반응식

HRID 622897 반응식
[NH2:1][CH2:2][CH:3]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH2:4][P:5](C(OCC)OCC)(=[O:9])[O:6]CC>Cl>[NH2:1][CH2:2][CH:3]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[CH2:4][P:5]([OH:9])[OH:6]

참가 물질

3

반응물 1

HCID 14362832Ethyl 3-amino-2-phenylpropyl(diethoxymethyl)phosphinate

생성물 1

HCID 100356503-Amino-2-phenylpropylphosphonous acid

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of 4.0 g of ethyl 3-amino-2-phenylpropyl(diethoxymethyl)phosphinate in 40 ml of 36% aqueous hydrochloric acid is heated to reflux for a period of 2 h. The reaction mixture is then allowed to cool to room temperature, concentrated under reduced pressure and co-evaporated twice with 20 ml of water under reduced pressure. The crude product is dissolved in 20 ml of water, washed twice with 20 ml of diethyl ether and the aqueous layer is then separated and evaporated under reduced pressure. The crude product is dissolved in 50 ml ethanol and 5 ml of propylene oxide is added dropwise. The precipitated solid is collected by filtration and dried to give 3-amino-2-phenylpropylphosphonous acid m.p. 228°-235° C., 31P=+24.3 ppm (D2O).

후처리

  1. temperatureto reflux for a period of 2 h
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe crude product is dissolved in 20 ml of water
  4. washwashed twice with 20 ml of diethyl ether
  5. customthe aqueous layer is then separated
  6. customevaporated under reduced pressure
  7. dissolutionThe crude product is dissolved in 50 ml ethanol
  8. addition5 ml of propylene oxide is added dropwise
  9. filtrationThe precipitated solid is collected by filtration
  10. customdried

출처 및 근거

ORD 기록
ord-a1936b106e85466e88263919d9623b2e
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772738

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