Hydrochloric Acid → L-homoalanin-4-yl(methyl)phosphinic acid hydrochloride

HRID 1649946

반응식

HRID 1649946 반응식
C([NH:4][C:5](=[CH:9][CH2:10][PH:11]([CH2:13]O)=[O:12])[C:6]([OH:8])=[O:7])(=O)C.[ClH:15].C[OH:17]>>[ClH:15].[ClH:15].[NH2:4][C@H:5]([C:6]([OH:8])=[O:7])[CH2:9][CH2:10][P:11]([CH3:13])(=[O:17])[OH:12]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 887Methanol2회HCID 178474815HCID 178474815, 화합물

생성물 2

HCID 313Hydrochloric AcidHCID 12701464L-homoalanin-4-yl(methyl)phosphinic acid hydrochloride수율 91.9%

실험 절차

0.0087 g (0.019 mmol) of chloronorbornadienerhodium(I) dimer and 0.022 g (0.053 mmol) of the compound Va are dissolved in 5 ml of methanol under an atmosphere of argon. The catalyst solution obtained is added under argon to a solution of 2.21 g (0.01 mol) of 2-acetamido-4-(hydroxymethylphosphinyl)-2-butenoic acid in 45 ml of methanol. The reaction vessel is evacuated, then hydrogenation is performed at a pressure of 3.0 bar. After a reaction time of 44 hours, the reaction vessel is depressurized, the reaction mixture evaporated down, the residue taken up in water and the precipitated catalyst separated off. As a result of adding an equivalent quantity of concentrated hydrochloric acid to the filtrate, a 6N hydrochloric acid solution is prepared which is boiled under reflux for 12 hours. After evaporating this solution down, 2.0 g (91.9% of theory) of L-homoalanin-4-yl(methyl)phosphinic acid hydrochloride is obtained as a white solid which is purified by recrystallization from an ethanol/water mixture.

후처리

  1. customThe catalyst solution obtained
  2. customThe reaction vessel is evacuated
  3. customAfter a reaction time of 44 hours
  4. customthe reaction mixture evaporated down
  5. customthe precipitated catalyst separated off
  6. customAs a result
  7. temperatureunder reflux for 12 hours
  8. customAfter evaporating this solution down

출처 및 근거

ORD 기록
ord-3b5954c9604849f1b2b973f418798d61
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04922006

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