Hydrochloric Acid → 3-Dimethylamino-1-(5-methyl-2-thienyl)-propan-1-one hydrochloride

HRID 236558

Reaktionsgleichung

Reaktionsgleichung von HRID 236558
[C:1]([C:4]1[S:5][C:6]([CH3:9])=[CH:7][CH:8]=1)(=[O:3])[CH3:2].[ClH:10].[CH3:11][NH:12][CH3:13].[CH2:14]=O.Cl>C(O)C>[ClH:10].[CH3:11][N:12]([CH3:14])[CH2:13][CH2:2][C:1]([C:4]1[S:5][C:6]([CH3:9])=[CH:7][CH:8]=1)=[O:3]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 836552-Acetyl-5-methylthiophene

Produkt 1

HCID 126434363-Dimethylamino-1-(5-methyl-2-thienyl)-propan-1-one hydrochlorideAusbeute 65,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Under a nitrogen atmosphere, a stirred solution of 10.0 grams (0.071 mole) of 2-acetyl-5-methylthiophene, 7.0 grams (0.086 mole) of dimethylamine hydrochloride, 2.5 grams of paraformaldehyde and 0.4 ml of concentrated hydrochloric acid in 10 ml of ethanol was heated under reflux for 16 hours. The reaction mixture was concentrated under reduced pressure to a residual solid. The solid was recrystallized from methanol-diethyl ether to give 10.9 grams of 3-dimethylamino-1-(5-methyl-2-thienyl)propan-1-one hydrochloride; m.p. 145°-147° C.

Aufarbeitung

  1. temperatureunder reflux for 16 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure to a residual solid
  3. customThe solid was recrystallized from methanol-diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-7533c9036b464e4a94d876df66df5f98
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04645777

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