Hydrochloric Acid → Hydroxyamfetamine

HRID 6729

Reaktionsgleichung

Reaktionsgleichung von HRID 6729
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](=O)[CH3:10])=[CH:4][CH:3]=1.C([O-])(=O)C.[NH4+].C([BH3-])#[N:18].[Na+].Cl>CO>[NH2:18][CH:9]([CH3:10])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([OH:1])=[CH:3][CH:4]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 70192744-Hydroxyphenylacetone

Produkt 1

HCID 3651HydroxyamfetamineAusbeute 56,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 4-hydroxyphenylacetone (0.5 g, Avocado, U.K.) and ammonium acetate (2.54 g, Aldrich, U.S.A.) in 10 mL methanol was added 0.17 g of sodium cyanoborohydride (Aldrich, U.S.A.). After stirring for 72 h at rt, concentrated hydrochloric acid was added dropwise until the solution reached pH 2. The solvent was evaporated and the resulting residue was dissolved in water, then extracted 3 times with diethyl ether. The aqueous layer was neutralized to pH 8 by the addition of potassium hydroxide and extracted with diethyl ether. The basic ether layer was dried over sodium sulfate and the solvent was removed in vacuo to give 0.23 g of 4-(2-amino-propyl)-phenol.

Aufarbeitung

  1. customThe solvent was evaporated
  2. dissolutionthe resulting residue was dissolved in water
  3. extractionextracted 3 times with diethyl ether
  4. additionThe aqueous layer was neutralized to pH 8 by the addition of potassium hydroxide
  5. extractionextracted with diethyl ether
  6. dry with materialThe basic ether layer was dried over sodium sulfate
  7. customthe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-66b12eb350804cde8d3d3a98c42becda
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07084154B2

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