Phosphorus sulfide (P2S5) → HCID 21256521, Verbindung

HRID 635794Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 635794
[CH2:1]([CH:3]1[C:8](=O)[NH:7][C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[O:4]1)[CH3:2].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:15]>N1C=CC=CC=1>[CH2:1]([CH:3]1[C:8](=[S:15])[NH:7][C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[O:4]1)[CH3:2]

Komponenten

4

Edukt 2

HCID 14817Phosphorus sulfide (P2S5)HCID 31555992-Ethyl-2H-benzo[b][1,4]oxazin-3(4H)-one

Produkt 1

HCID 21256521HCID 21256521, VerbindungAusbeute 532,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

0.25 g of 2-ethyl-1,4-benzoxazin-3-one is stirred in 2 ml of pyridine with 95 mg of phosphorus pentasulfide. The reaction is completed by reflux-boiling. It is poured onto water, extracted with ethyl acetate, and the organic phase is washed with brine. It is dried with magnesium sulfate and concentrated by evaporation. After column chromatography with hexane/ethyl acetate, 220 mg of product results.

Aufarbeitung

  1. temperatureby reflux-boiling
  2. additionIt is poured onto water
  3. extractionextracted with ethyl acetate
  4. washthe organic phase is washed with brine
  5. dry with materialIt is dried with magnesium sulfate
  6. concentrationconcentrated by evaporation

Quellen und Nachweise

ORD-Eintrag
ord-97f59d314a304465accf2e88423a266d
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06191127B1

Notizen zur Reaktion

Wird geladen…