Hydrochloric Acid → HCID 20289969, Verbindung

HRID 1856102Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1856102
[CH3:1][C:2]1[CH:26]=[CH:25][C:5]([O:6][CH:7]([C:9]2[S:13][C:12]([NH:14][C:15](=[O:24])[N:16]([CH2:18][CH:19](OC)[O:20]C)[CH3:17])=[N:11][N:10]=2)[CH3:8])=[CH:4][CH:3]=1.Cl>O>[CH3:1][C:2]1[CH:26]=[CH:25][C:5]([O:6][CH:7]([C:9]2[S:13][C:12]([N:14]3[CH:19]([OH:20])[CH2:18][N:16]([CH3:17])[C:15]3=[O:24])=[N:11][N:10]=2)[CH3:8])=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 20289954HCID 20289954, Verbindung

Produkt 1

HCID 20289969HCID 20289969, VerbindungAusbeute 104 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture containing 3.5 grams of the 3-[5-[1-(4-methylphenoxy)ethyl]-1,3,4-thiadiazol-2-yl]-1-methyl-(2,2-dimethoxyethyl)urea (prepared above), 150 milliliters of water and 1.5 milliliters of concentrated hydrochloric acid (HCl) was refluxed for 25 minutes, then cooled with formation of an oil. The oil was extracted with chloroform, and the chloroform extract was dried over magnesium sulfate (MgSO4), filtered and topped on a roto-vac at 70° C. to yield 3.2 grams of an orange oil. It was dissolved in diethylether and heated with formation of crystals which were filtered off and dried in a vacuum oven at 70° C. to 1.8 grams of ivory crystals of [5-[1-(4-methylphenoxy)ethyl]-1,3,4-thiadiazol-2-yl]-1-methyl-4-hydroxy-2-imidazolidinone, (melting point 126°-128° C.).

Aufarbeitung

  1. temperaturewas refluxed for 25 minutes
  2. temperaturecooled with formation of an oil
  3. extractionThe oil was extracted with chloroform
  4. extractionthe chloroform extract
  5. dry with materialwas dried over magnesium sulfate (MgSO4)
  6. filtrationfiltered
  7. customtopped on a roto-vac at 70° C.

Quellen und Nachweise

ORD-Eintrag
ord-4de323233b67494f9419979238fcab67
Quelldatensatz
uspto-grants-1980_08
Patentnummer
US04218236

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