Hydrochloric Acid → 1-Amino-4-methylpentan-2-one hydrochloride

HRID 1670529Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1670529
[CH3:1][CH:2]([CH3:18])[CH2:3][C:4](=[O:17])[CH2:5][N:6]1C(=O)C2C(=CC=CC=2)C1=O.[ClH:19]>C(O)(=O)C.O>[ClH:19].[NH2:6][CH2:5][C:4](=[O:17])[CH2:3][CH:2]([CH3:18])[CH3:1]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 70388412-(4-methyl-2-oxopentyl)-1H-isoindole-1,3(2H)-dione

Produkt 1

HCID 137017551-Amino-4-methylpentan-2-one hydrochlorideAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Slurry 2-(4-methyl-2-oxo-pentyl)-isoindole-1,3-dione (2.8 g, 11.4 mmol) in concentrated HCl (18 mL), glacial acetic acid (16 mL) and water (13 mL). Stir the mixture at reflux for 16 h. Cool to room temperature and pour the solution onto ice (25 mL). Filter off the solids, wash the filtrate with cold water (20 mL) and concentrate in vacuo to a solid. Recrystallize the solid in ethanol (15 mL) and diethyl ether (50 mL). Decant off the solvent and dry the white paste under reduced pressure to obtain the desired intermediate as a white solid (1.4 g, 81%).

Aufarbeitung

  1. temperatureat reflux for 16 h
  2. additionpour the solution onto ice (25 mL)
  3. filtrationFilter off the solids
  4. washwash the filtrate with cold water (20 mL)
  5. concentrationconcentrate in vacuo to a solid
  6. customRecrystallize the solid in ethanol (15 mL)
  7. customDecant off the solvent
  8. customdry the white paste under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f1bb7b21e6ea49529d86b787c1a95764
Quelldatensatz
uspto-grants-2011_08
Patentnummer
US07994163B2

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