HCID 53980706, Verbindung → 60201-60-7

HRID 1679672Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1679672
Cl[CH2:2][CH2:3][NH:4][C:5]([N:7]([C:9]1[CH:14]=[CH:13][C:12]([C:15]([OH:24])([C:20]([F:23])([F:22])[F:21])[C:16]([F:19])([F:18])[F:17])=[CH:11][CH:10]=1)[CH3:8])=[O:6]>CO.O>[F:17][C:16]([F:19])([F:18])[C:15]([C:12]1[CH:13]=[CH:14][C:9]([N:7]([C:5]2[O:6][CH2:2][CH2:3][N:4]=2)[CH3:8])=[CH:10][CH:11]=1)([OH:24])[C:20]([F:23])([F:22])[F:21]

Komponenten

4

Edukt 1

HCID 53980706HCID 53980706, Verbindung

Produkt 1

HCID 2131494660201-60-7Ausbeute 86,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Dissolve 10.0 g (26 m. mole) of N-(2-chloroethyl)-N'-[4-(hexafluoro-2-hydroxy-2-propyl)phenyl]-N'-methyl-urea in a mixture of 50 ml of methanol and 100 ml of water. Heat for 1 hour on a steam bath. Concentrate, and partition between 1N aqueous sodium bicarbonate solution and ether (diethyl) and then extract with 200 ml of 1N hydrochloric acid. Add sodium bicarbonate and then extract with 200 ml of ether. Dry the ether extract and concentrate to obtain 7.8 g of the title compound as a white solid, m.p. 188°-190° C. The salts may be prepared by standrad techniques such as by treatment of a solution of the free base in a suitable organic solvent, e.g. ether, with the desired acid, e.g. hydrochloric, and then filtering off the precipitated salt. The hydrochloride salt melts at 147°-149° C.

Aufarbeitung

  1. temperatureHeat for 1 hour on a steam bath
  2. concentrationConcentrate
  3. custompartition between 1N aqueous sodium bicarbonate solution and ether (diethyl)
  4. extractionextract with 200 ml of 1N hydrochloric acid
  5. extractionAdd sodium bicarbonate and then extract with 200 ml of ether
  6. dry with materialDry the ether
  7. extractionextract
  8. concentrationconcentrate

Quellen und Nachweise

ORD-Eintrag
ord-353763ece87343c9be906e14b880d9a6
Quelldatensatz
uspto-grants-1978_03
Patentnummer
US04081547

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