Oxirane, [[4-[2-(2-methylpropoxy)ethoxy]phenoxy]methyl]- → HCID 20222108, Verbindung

HRID 980166Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 980166
[CH3:1][CH:2]([CH3:19])[CH2:3][O:4][CH2:5][CH2:6][O:7][C:8]1[CH:18]=[CH:17][C:11]([O:12][CH2:13][CH:14]2[O:16][CH2:15]2)=[CH:10][CH:9]=1.[NH2:20][CH2:21][CH2:22][NH:23][C:24]([N:26]([CH3:28])[CH3:27])=[O:25]>C(O)(C)C>[CH3:27][N:26]([CH3:28])[C:24]([NH:23][CH2:22][CH2:21][NH:20][CH2:15][CH:14]([OH:16])[CH2:13][O:12][C:11]1[CH:17]=[CH:18][C:8]([O:7][CH2:6][CH2:5][O:4][CH2:3][CH:2]([CH3:19])[CH3:1])=[CH:9][CH:10]=1)=[O:25]

Komponenten

4

Edukt 2

HCID 10635469Oxirane, [[4-[2-(2-methylpropoxy)ethoxy]phenoxy]methyl]-HCID 20383014N'-(2-Aminoethyl)-N,N-dimethylurea

Produkt 1

HCID 20222108HCID 20222108, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

8 g of 3-(4-(2-(2-methylpropoxy)ethoxy)phenoxy)-1,2-epoxypropane and 14 g of N-2-aminoethyl-N',N'-dimethylurea was warmed (60°-70° C.) in 150 ml of isopropanol over night. The mixture was evaporated and the residue dissolved in ethyl acetate. The ethyl acetate phase was washed with water (twice), fresh water was then added and pH lowered to 5 with hydrochloric acid. Fresh ethyl acetate was then added to the water phase and pH was rised to 9.5. The organic phase was separated off, dried, and evaporated. The residue was recrystallized from a small amount of ethyl acetate. Yield 3 g. M.p. 75° C. (base). The structure was determined using NMR-analysis.

Aufarbeitung

  1. customThe mixture was evaporated
  2. dissolutionthe residue dissolved in ethyl acetate
  3. washThe ethyl acetate phase was washed with water (twice), fresh water
  4. additionwas then added
  5. additionFresh ethyl acetate was then added to the water phase and pH
  6. customThe organic phase was separated off
  7. customdried
  8. customevaporated
  9. customThe residue was recrystallized from a small amount of ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-54c1b940729641c49eefa387cfa091b9
Quelldatensatz
uspto-grants-1987_01
Patentnummer
US04636501

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