HCID 54145704, 화합물 → 3-{N-[1-(3,4-dichlorophenyl)ethyl]amino}-2(S)-hydroxy-propyl(cyclohexylmethyl)phosphinic acid hydrochloride

HRID 1492967노트

반응식

HRID 1492967 반응식
C([O:3][P:4]([CH2:13][C@@H:14]([OH:27])[CH2:15][NH:16][CH:17]([C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[C:21]([Cl:26])[CH:20]=1)[CH3:18])([CH2:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)=[O:5])C>Cl>[ClH:25].[Cl:26][C:21]1[CH:20]=[C:19]([CH:17]([NH:16][CH2:15][C@H:14]([OH:27])[CH2:13][P:4]([CH2:6][CH:7]2[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)(=[O:3])[OH:5])[CH3:18])[CH:24]=[CH:23][C:22]=1[Cl:25]

참가 물질

3

반응물 1

HCID 54145704HCID 54145704, 화합물

생성물 1

HCID 677418273-{N-[1-(3,4-dichlorophenyl)ethyl]amino}-2(S)-hydroxy-propyl(cyclohexylmethyl)phosphinic acid hydrochloride

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of 4.1 g of 3-{N-[1-(3,4-dichlorophenyl)ethyl]amino}-2(S)-hydroxy-propyl(cyclohexylmethyl)phosphinic acid ethyl ester in 30 ml of 5N hydrochloric acid is heated at reflux for 24 hours, during which time two phases are formed. The reaction mixture is cooled to room temperature and the solvent is removed under reduced pressure; the residue is taken up in absolute ethanol and the residual water is distilled off azeotropically. The white solid that remains behind is crystallised from isopropanol, yielding 3-{N-[1-(3,4-dichlorophenyl)ethyl]amino}-2(S)-hydroxy-propyl(cyclohexylmethyl)phosphinic acid hydrochloride having a melting point of 174°-180°.

후처리

  1. temperatureat reflux for 24 hours, during which time two phases
  2. customare formed
  3. customthe solvent is removed under reduced pressure
  4. distillationthe residual water is distilled off azeotropically
  5. customThe white solid that remains behind is crystallised from isopropanol

출처 및 근거

ORD 기록
ord-5b8a6a5ce0cc42929fdbaeef372f1340
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05376684

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