Hydrochloric Acid → HCID 70507303, Verbindung

HRID 358213

Reaktionsgleichung

Reaktionsgleichung von HRID 358213
[ClH:1].[NH:2]1[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.[C:8]([C:12]1[CH:17]=[CH:16][C:15]([C:18](=[O:21])[CH2:19][CH3:20])=[CH:14][CH:13]=1)([CH3:11])([CH3:10])[CH3:9].[CH2:22]=O.Cl>C(O)C>[ClH:1].[C:8]([C:12]1[CH:13]=[CH:14][C:15]([C:18](=[O:21])[CH:19]([CH3:22])[CH2:20][N:2]2[CH2:7][CH2:6][O:5][CH2:4][CH2:3]2)=[CH:16][CH:17]=1)([CH3:11])([CH3:10])[CH3:9]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 197884Morpholine, hydrochloride (1:1)HCID 5952814'-(tert-Butyl)propiophenone

Produkt 1

HCID 70507303HCID 70507303, VerbindungAusbeute 61,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

37.07 g (0.3 mole) of morpholine hydrochloride, 57.1 g (0.3 mole) of p-tert.-butyl-propiophenone and 15.01 g (0.5 mole) of paraformaldehyde were heated under reflux in 150 ml of ethanol for 1 hour. After adding 0.5 ml of concentrated hydrochloric acid, the reaction mixture was stirred under reflux for a further 15 hours. It was then concentrated, the residue was taken up in chloroform, the chloroform mixture was washed twice with water and the organic phase was dried over sodium sulphate and concentrated. The crystalline residue was suspended in hot ethyl acetate, filtered off and dried. 60 g (61.5% of theory) of p-tert.-butyl-2-methyl-3-morpholin-4-yl-propiophenone hydrochloride of melting point 189° to 91° C. were obtained.

Aufarbeitung

  1. temperatureunder reflux for a further 15 hours
  2. concentrationIt was then concentrated
  3. washthe chloroform mixture was washed twice with water
  4. dry with materialthe organic phase was dried over sodium sulphate
  5. concentrationconcentrated
  6. filtrationfiltered off
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-62a2654f9dba4e319efe497df3f64a86
Quelldatensatz
uspto-grants-1984_08
Patentnummer
US04465678

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