Lithium hydroxide, monohydrate → HCID 10370074, Verbindung

HRID 497143

Reaktionsgleichung

Reaktionsgleichung von HRID 497143
C([O:3][C:4]([CH:6]1[CH2:11][N:10]([CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9][CH2:8][N:7]1[C:25](=[O:40])[CH2:26][CH:27]([C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:5])C.O[Li].O>C1COCC1.CO.O>[CH:12]([N:10]1[CH2:9][CH2:8][N:7]([C:25](=[O:40])[CH2:26][CH:27]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH:6]([C:4]([OH:5])=[O:3])[CH2:11]1)([C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

Komponenten

4

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 103247844-Benzhydryl-1-(3,3-diphenyl-propionyl)-piperazine-2-carboxylic acid ethyl ester

Produkt 1

HCID 10370074HCID 10370074, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21892291Methanol tetrahydrofuran waterLösungsmittel

Versuchsvorschrift

A mixture of 4-Benzhydryl-1-(3,3-diphenyl-propionyl)-piperazine-2-carboxylic acid ethyl ester (0.51 g, 0.957 mmol), and LiOH.H2O (0.12 g, 2.87 mmol) in THF/MeOH/H2O (15:5:5) was stirred at room temperature for two days. The solvent was evaporated under reduced pressure, the residue was dissolved in water, acidified with 1N HCl to pH 3. The product was extracted with EtOAc, dried with MgSO4, and evaporated under reduced pressure. The product was purified by column chromatography (CH2Cl2:MeOH 15:1) to give the title compound in 95% yield.

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in water
  3. extractionThe product was extracted with EtOAc
  4. dry with materialdried with MgSO4
  5. customevaporated under reduced pressure
  6. customThe product was purified by column chromatography (CH2Cl2:MeOH 15:1)

Quellen und Nachweise

ORD-Eintrag
ord-fc8c15f88e2840bbb6c363573abb17ba
Quelldatensatz
uspto-grants-2005_09
Patentnummer
US06949554B2

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