Methylamine → HCID 20186775, Verbindung

HRID 2309008Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2309008
[C:1]([CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH:14]([NH:16][CH2:17][CH:18]([O:26][CH2:27][CH2:28][OH:29])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)[CH3:15])=[CH:9][CH:8]=1)(OC)=[O:2].[CH3:30][NH2:31]>C(O)C>[ClH:25].[CH3:30][NH:31][C:1]([CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH:14]([NH:16][CH2:17][CH:18]([O:26][CH2:27][CH2:28][OH:29])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)[CH3:15])=[CH:9][CH:8]=1)=[O:2]

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 21285459HCID 21285459, Verbindung

Produkt 1

HCID 20186775HCID 20186775, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of N-[2-(4-carbomethoxymethoxyphenyl)-1-methylethyl]-2-(2-hydroxyethoxy)-2-(3-chlorophenyl)ethanamine (4.0 g) and 33% methylamine in ethanol (50 ml) was heated under reflux for 1.5 h. The mixture was evaporated under reduced pressure and the residue converted to its hydrochloride by addition of ethereal hydrogen chloride. Recrystallisation from ethyl acetate-methanol gave the title compound, mp. 117°-121° C. as a 56:44 mixture of diastereoisomers.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 1.5 h
  3. customThe mixture was evaporated under reduced pressure
  4. additionthe residue converted to its hydrochloride by addition of ethereal hydrogen chloride
  5. customRecrystallisation from ethyl acetate-methanol

Quellen und Nachweise

ORD-Eintrag
ord-a3d7d059f30744e193bf503e17563581
Quelldatensatz
uspto-grants-1987_09
Patentnummer
US04692465

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