Sulfate Ion → N-(2-((2-hydroxy-3-(4-(2-methoxyethoxy)phenoxy)propyl)amino)ethyl)-4-morpholinecarboxamide

HRID 980159Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 980159
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:16]=[CH:15][C:9]([O:10][CH2:11][CH:12]2[O:14][CH2:13]2)=[CH:8][CH:7]=1.S([O-])([O-])(=O)=O.[NH2:22][CH2:23][CH2:24][NH:25][C:26]([N:28]1[CH2:33][CH2:32][O:31][CH2:30][CH2:29]1)=[O:27].C([O-])([O-])=O.[K+].[K+]>CC(O)C>[OH:14][CH:12]([CH2:11][O:10][C:9]1[CH:15]=[CH:16][C:6]([O:5][CH2:4][CH2:3][O:2][CH3:1])=[CH:7][CH:8]=1)[CH2:13][NH:22][CH2:23][CH2:24][NH:25][C:26]([N:28]1[CH2:33][CH2:32][O:31][CH2:30][CH2:29]1)=[O:27]

Komponenten

6

Edukt 4

HCID 1117Sulfate IonHCID 11430Potassium CarbonateHCID 11041198N-(2-Aminoethyl)-4-morpholinecarboxamideHCID 126215491-(2,3-Epoxypropoxy)-4-(2-methoxyethoxy)benzene

Produkt 1

HCID 20222106N-(2-((2-hydroxy-3-(4-(2-methoxyethoxy)phenoxy)propyl)amino)ethyl)-4-morpholinecarboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

4 g of 3-(4-(2-methoxyethoxy)phenoxy)-1,2-epoxypropane, 5.8 g of the sulphate of N-2-aminoethyl-4-morpholinecarboxamide, and 5.8 g of K2CO3 were refluxed in 2-propanol for 2 days. The mixture was filtered and concentrated in vacuo. The residue was dissolved in methylene chloride and washed with H2O. The organic phase was dried over Na2SO4, filtered and evaporated. The product was recrystallized from ethyl acetate. Yield 2.3 g. Melting point 69° C. (base). The structure was determined using NMR and equivalent weight.

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in methylene chloride
  4. washwashed with H2O
  5. dry with materialThe organic phase was dried over Na2SO4
  6. filtrationfiltered
  7. customevaporated
  8. customThe product was recrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-ef615be404514c78b21cfad46faf6846
Quelldatensatz
uspto-grants-1987_01
Patentnummer
US04636501

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