Phosphorus oxychloride → HCID 86722242, Verbindung

HRID 869393Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 869393
O[C:2]1[CH:7]=[C:6]([C:8]2[N:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[S:11][CH:12]=2)[N:5]=[C:4]2[C:16]3[C:22]([Cl:23])=[C:21]([O:24][CH3:25])[CH:20]=[CH:19][C:17]=3[O:18][C:3]=12.O=P(Cl)(Cl)[Cl:28]>>[Cl:28][C:2]1[CH:7]=[C:6]([C:8]2[N:9]=[C:10]([CH:13]([CH3:15])[CH3:14])[S:11][CH:12]=2)[N:5]=[C:4]2[C:16]3[C:22]([Cl:23])=[C:21]([O:24][CH3:25])[CH:20]=[CH:19][C:17]=3[O:18][C:3]=12

Komponenten

3

Versuchsvorschrift

The crude 10C (8.75 g, 23.34 mmol) was added to POCl3 (200 mL) The mixture was refluxed for 2 hours. TLC monitored the reaction. After the reaction completed, POCl3 was evaporated under reduced pressure. The residue was poured into crushed ice under stirring. The yellow solids were collected by filtration and purified by flash chromatography to give product M10 (0.66 g).

Aufarbeitung

  1. temperaturewas refluxed for 2 hours
  2. customthe reaction
  3. customPOCl3 was evaporated under reduced pressure
  4. additionThe residue was poured
  5. custominto crushed ice
  6. filtrationThe yellow solids were collected by filtration
  7. custompurified by flash chromatography
  8. customto give product M10 (0.66 g)

Quellen und Nachweise

ORD-Eintrag
ord-a8a8e91967864ef4b21bc3073a0eac08
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969373B2

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