Morpholine → 2-Methyl-2-morpholino-1-(4-piperidinophenyl)-propan-1-one

HRID 1885651Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1885651
[CH3:1][C:2]1([CH3:19])O[C:3]1([O:17]C)[C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1.[NH:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1>C1(C)C=CC=CC=1>[CH3:19][C:2]([N:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1)([CH3:1])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1)=[O:17]

Komponenten

4

Edukt 2

HCID 8083Morpholine2×HCID 198794483,3-Dimethyl-2-methoxy-2-(4-piperidinophenyl)-oxirane

Produkt 1

HCID 198794392-Methyl-2-morpholino-1-(4-piperidinophenyl)-propan-1-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

12.1 g (46.3 mmol) of 3,3-dimethyl-2-methoxy-2-(4-piperidinophenyl)-oxirane and 26.1 g (0.30 mol) of morpholine are added together, and the mixture is heated to the refluxing temperature (about 130° C.). After 6 hours the mixture is cooled down and the morpholine is dissolved off under reduced pressure. The residue is taken up in toluene and is extracted with dilute hydrochloric acid. The hydrochloric acid solution is rendered alkaline and is extracted with toluene. The toluene solution is dried with K2CO3 and concentrated. The residue is recrystallised from methanol. Melting point 159°-162° C.

Aufarbeitung

  1. temperatureAfter 6 hours the mixture is cooled down
  2. extractionis extracted with dilute hydrochloric acid
  3. extractionis extracted with toluene
  4. dry with materialThe toluene solution is dried with K2CO3
  5. concentrationconcentrated
  6. customThe residue is recrystallised from methanol

Quellen und Nachweise

ORD-Eintrag
ord-bd986129cd9e4a40a670d5dace2405db
Quelldatensatz
uspto-grants-1992_09
Patentnummer
US05145885

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