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

HRID 1440680ノート

反応式

HRID 1440680 の反応式
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]

参加物

3

反応物 1

HCID 54145704HCID 54145704、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-bd2c052e52ca44f09fa6283377613c74
出典データセット
uspto-grants-1996_03
特許番号
US05500418

反応ノート

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