Hydrochloric Acid → HCID 13020006, Verbindung

HRID 1277818Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1277818
[O:1]([C:8]1[CH:13]=[CH:12][C:11]([NH:14][C:15]([N:17]([CH2:19][CH:20](OC)OC)[CH3:18])=[O:16])=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>O>[CH3:18][N:17]1[CH:19]=[CH:20][N:14]([C:11]2[CH:10]=[CH:9][C:8]([O:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)=[CH:13][CH:12]=2)[C:15]1=[O:16]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 13020004HCID 13020004, Verbindung

Produkt 1

HCID 13020006HCID 13020006, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

N-(4-Phenoxyphenyl)-N'-(2,2-dimethoxyethyl)-N'-methylurea (5.0 grams, 0.015 mole), water (30 ml) and concentrated hydrochloric acid (3 ml) were charged into a glass reaction vessel fitted with a mechanical stirrer thermometer and condenser. The reaction mixture was refluxed for a period of about 15 minutes, cooled and extracted with ethyl acetate. The ethyl acetate solution was washed with dilute aqueous sodium bicarbonate and with portions of water and dried. The ethyl acetate was removed by mild warming under reduced pressure to yield a residue. This was recrystallized from ethyl acetate to yield the desired product 1-methyl-3-(4-phenoxyphenyl)-4-imidazolin-2-one as a solid having a melting point of 112° C.

Aufarbeitung

  1. customfitted with a mechanical stirrer thermometer and condenser
  2. temperatureThe reaction mixture was refluxed for a period of about 15 minutes
  3. temperaturecooled
  4. extractionextracted with ethyl acetate
  5. washThe ethyl acetate solution was washed with dilute aqueous sodium bicarbonate and with portions of water
  6. customdried
  7. customThe ethyl acetate was removed
  8. temperatureby mild warming under reduced pressure
  9. customto yield a residue
  10. customThis was recrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-330ba492c03448bc856b722bf356a075
Quelldatensatz
uspto-grants-1981_07
Patentnummer
US04279637

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