Phosphorus oxychloride → HCID 21846021, Verbindung

HRID 619092

Reaktionsgleichung

Reaktionsgleichung von HRID 619092
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8](O)=O.[NH2:11][NH:12][C:13]([NH2:15])=[S:14].O1CCOCC1.O=P(Cl)(Cl)Cl>C(Cl)Cl.O>[NH2:15][C:13]1[S:14][C:8]([CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][Br:1])=[N:11][N:12]=1

Komponenten

7

Edukt 4

HCID 24813Phosphorus oxychlorideHCID 312751,4-DioxaneHCID 1217237-Bromoheptanoic acidHCID 2723789Thiosemicarbazide

Produkt 1

HCID 21846021HCID 21846021, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

5 g of 7-bromoheptanoic acid and 2.17 g of thiosemicarbazide were introduced into 50 ml of dioxane at 90° C. and, at this temperature, 4.0 g of POCl3 were added dropwise. The mixture was then stirred at 90° C. for 1 hour. Then water was added to the mixture, and extraction 3 times with methylene chloride, drying over MgSO4 and concentration were carried out. 6.1 g (=96% yield) of product were obtained as residue.

Aufarbeitung

  1. additionwere added dropwise
  2. dry with materialdrying over MgSO4 and concentration
  3. custom6.1 g (=96% yield) of product were obtained as residue

Quellen und Nachweise

ORD-Eintrag
ord-9902cadbef08472c8438efd2e1fc0ba1
Quelldatensatz
uspto-grants-1999_09
Patentnummer
US05958923

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