Water → HCID 19974642, Verbindung

HRID 1451641Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1451641
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11]1[CH:19]=[CH:18][C:17]([S:20][CH3:21])=[CH:16][C:12]=1[C:13]([OH:15])=[O:14])([OH:3])=O.O>P(Cl)(Cl)(Cl)=O>[CH3:21][S:20][C:17]1[CH:16]=[C:12]([C:13]([OH:15])=[O:14])[C:11]2[NH:10][C:5]3[C:4](=[CH:9][CH:8]=[CH:7][CH:6]=3)[C:1](=[O:3])[C:19]=2[CH:18]=1

Komponenten

4

Edukt 2

HCID 962WaterHCID 19974595HCID 19974595, Verbindung

Produkt 1

HCID 19974642HCID 19974642, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813Phosphorus oxychlorideLösungsmittel

Versuchsvorschrift

The product of part (i) above (2 g) in phosphorus oxychloride (6 ml) was heated at reflux for 1 h. The solution was then cooled (to 0°), and water (15 ml) was added slowly. The mixture was then heated at 100° for 10 min and then poured onto cracked ice. The resulting precipitate was filtered off, washed with water, and crystallised from methanol to give the title compound (1.6 g). IR includes peaks at 1690 cm-1 (CO2H) and 1620 cm-1 (CO).

Aufarbeitung

  1. temperatureat reflux for 1 h
  2. additionwas added slowly
  3. temperatureThe mixture was then heated at 100° for 10 min
  4. additionpoured
  5. filtrationThe resulting precipitate was filtered off
  6. washwashed with water
  7. customcrystallised from methanol

Quellen und Nachweise

ORD-Eintrag
ord-76c77db7d62247a1b4d752a6666c52e5
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05604237

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