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Hydrochloric Acid → HCID 20225207, Verbindung

HRID 1249201
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1249201
Cl.[C:2]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH:15]([NH:17][CH2:18][CH:19]([O:27][CH3:28])[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=2)[CH3:16])=[CH:10][CH:9]=1)(OC)=[O:3].[CH3:29][NH2:30].Cl>CO.[Cl-].[Na+]>[ClH:26].[CH3:29][NH:30][C:2]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH:15]([NH:17][CH2:18][CH:19]([O:27][CH3:28])[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=2)[CH3:16])=[CH:10][CH:9]=1)=[O:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 6329Methylamine3×HCID 20225212HCID 20225212, Verbindung

Produkt 1

HCID 20225207HCID 20225207, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 5234Sodium Chloride
Lösungsmittel

Versuchsvorschrift

To a solution of N-[2-(4-carbomethoxymethoxyphenyl)-1-methylethyl]-2-methoxy-2-(3-chlorophenyl)ethanamine hydrochloride (0.63 g, diastereoisomeric ratio 92:8) in methanol was added 5 ml of a 30% aqueous solution of methylamine. This mixture was boiled under reflux for 6 hours during which time 3 further 5 ml portions of the methylamine solution were added. The solution was cooled to room temperature, a further 5 ml of methylamine solution added and the reaction mixture allowed to stand at room temperature overnight. After diluting with saturated sodium chloride solution the mixture was extracted with dichloromethane, washed with saturated sodium chloride solution, dried (magnesium sulphate), filtered and evaporated to give an oil which was converted to its hydrochloride salt by addition of ethereal hydrogen chloride. Recrystallisation from methanol-ethyl acetate gave the title compound, mp 217°-9° C., as single diastereoisomer.

Aufarbeitung

  1. additionwere added
  2. extractionwas extracted with dichloromethane
  3. washwashed with saturated sodium chloride solution
  4. dry with materialdried (magnesium sulphate)
  5. filtrationfiltered
  6. customevaporated
  7. customto give an oil which
  8. customRecrystallisation from methanol-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-3a2237a7705d44a1b2938630a7c5200b
Quelldatensatz
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04629737

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