Hydrochloric Acid → 4-(Azetidin-3-yl)morpholine dihydrochloride

HRID 1066065Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1066065
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH2:9]2)C=CC=CC=1.[ClH:24]>[OH-].[Pd+2].[OH-].C(O)C>[ClH:24].[ClH:24].[O:15]1[CH2:16][CH2:17][N:12]([CH:10]2[CH2:11][NH:8][CH2:9]2)[CH2:13][CH2:14]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 211837864-[1-(Diphenylmethyl)azetidin-3-yl]morpholine

Produkt 1

HCID 220613264-(Azetidin-3-yl)morpholine dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9942167Palladium hydroxideKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 1-diphenylmethyl-3-morpholinoazetidine (see PREPARATION 12) (18.6 g, 60.4 mmol), palladium hydroxide (2 g), ethanol (200 ml) and 1N aqueous hydrochloric acid solution (52 ml) was stirred under an atmosphere of hydrogen at 345 kPa (50 p.s.i.) for three days. The catalyst was then removed by filtration and the filtrate evaporated to dryness. Addition of dichloromethane (100 ml) to the residue and trituration yielded a solid which was recrystallised from methanol to give the title compound (10.2 g) as a crystalline solid.

Aufarbeitung

  1. customThe catalyst was then removed by filtration
  2. customthe filtrate evaporated to dryness
  3. additionAddition of dichloromethane (100 ml) to the residue and trituration
  4. customyielded a solid which
  5. customwas recrystallised from methanol

Quellen und Nachweise

ORD-Eintrag
ord-ac252939b8064dddbbb807dbbd727aa5
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06242438B1

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