Hydrochloric Acid → HCID 22063454, Verbindung

HRID 1666165Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1666165
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH:13]C(=O)C)([CH3:12])[CH3:11])=[CH:5][CH:4]=1)[CH3:2].[OH-].[K+].Cl.C(OCC)C>C(O)CO.C(#N)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH2:13])([CH3:12])[CH3:11])=[CH:5][CH:4]=1)[CH3:2]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14797Potassium HydroxideHCID 22063473HCID 22063473, Verbindung

Produkt 1

HCID 22063454HCID 22063454, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 174Ethylene GlycolLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

16.3 g (74 mmol) of N-[2-(4-ethylphenyl)-1,1-dimethylethyl]acetamide and 8.0 g of potassium hydroxide are refluxed for 15 hours in 60 mL ethylene glycol. The reaction mixture is combined with ice water and extracted three times with diethyl ether. The combined organic phases are washed with water, dried with sodium sulfate, and freed from solvent. To prepare the hydrochloride, the crude product is dissolved in acetonitrile and ethereal hydrochloric acid and diethyl ether are added successively. The solid precipitated is suction filtered and dried. Yield: 11.0 g (69%, hydrochloride); melting point 165° C.-167° C.

Aufarbeitung

  1. extractionextracted three times with diethyl ether
  2. washThe combined organic phases are washed with water
  3. dry with materialdried with sodium sulfate
  4. customTo prepare the hydrochloride
  5. customThe solid precipitated
  6. filtrationfiltered
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-673d2240aed54f2da0d14f5dee1637ae
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08044046B2

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