Hydrochloric Acid → 4-(4-Benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid

HRID 1619965Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1619965
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=[O:25])[CH:16]([CH:18](C(O)=O)[C:19]([OH:21])=[O:20])[CH3:17])=[CH:11][C:10]=1[OH:26])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)COCCO.COC.C(OC(C)C)(C)C.Cl>O>[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=[O:25])[CH:16]([CH3:17])[CH2:18][C:19]([OH:21])=[O:20])=[CH:11][C:10]=1[OH:26])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 7914Diisopropyl EtherHCID 212256572-(2-Hydroxyethoxy)ethanol;methoxymethaneHCID 674670302-[2-(4-Benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid

Produkt 1

HCID 674661774-(4-Benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

78.9 g (220.8 mmol) 2-[2-(4-benzylamino-3-hydroxy-phenyl)-1-methyl-2-oxo-ethyl]-malonic acid are combined with 200 ml diethyleneglycol-dimethylether and stirred for 3 h at 140° C. The mixture is combined with water and diisopropylether, then it is adjusted with 6N hydrochloric acid to pH=2 and extracted with DCM. The org. phase is separated off and dried on magnesium sulphate, then the solv. is eliminated by rotary evaporation i.V., the residue is stirred with diisopropylether and filtered off.

Aufarbeitung

  1. extractionextracted with DCM
  2. customphase is separated off
  3. customdried on magnesium sulphate
  4. stirring, the residue is stirred with diisopropylether
  5. filtrationfiltered off

Quellen und Nachweise

ORD-Eintrag
ord-c9736f84cf7f46008f3683e08e20853f
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772323B2

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