Phosphorus oxychloride → HCID 15907971, Verbindung

HRID 2224044Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2224044
P(Cl)(Cl)(Cl)=O.[C:6]([C@@:8]12[CH2:25][CH2:24][C:23]3[CH:22]=[C:21]([O:26][CH3:27])[CH:20]=[CH:19][C:18]=3[C@H:17]1[CH:16](O)[CH2:15][C@@:13]1([CH3:14])[C@H:9]2[CH2:10][CH2:11][C@@H:12]1[O:29][CH:30]1[CH2:35][CH2:34][CH2:33][CH2:32][O:31]1)#[N:7].C(=O)(O)[O-].[Na+]>N1C=CC=CC=1>[C:6]([C@@:8]12[CH2:25][CH2:24][C:23]3[CH:22]=[C:21]([O:26][CH3:27])[CH:20]=[CH:19][C:18]=3[C:17]1=[CH:16][CH2:15][C@@:13]1([CH3:14])[C@H:9]2[CH2:10][CH2:11][C@@H:12]1[O:29][CH:30]1[CH2:35][CH2:34][CH2:33][CH2:32][O:31]1)#[N:7]

Komponenten

5

Edukt 3

HCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 69105088HCID 69105088, Verbindung

Produkt 1

HCID 15907971HCID 15907971, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

27.6 ml of phosphorus oxychloride was added in drops to a solution of 27.6 g of 4 in 275 ml of pyridine at a temperature of 0-5° C., and it was stirred for another 1.5 hours at this temperature. Then, the mixture was moved into a dropping funnel and added in drops to an ice-cooled, saturated sodium bicarbonate solution. Then, it was extracted with dichloromethane, the collected organic phases were washed with brine, dried on magnesium sulfate, and the solvent was removed in a vacuum. In this way, 23.5 g (89%) of almost colorless, foamy 5 was obtained, which was used without further purification in the next stage.

Aufarbeitung

  1. customThen, the mixture was moved into a dropping funnel
  2. temperaturecooled
  3. extractionThen, it was extracted with dichloromethane
  4. washthe collected organic phases were washed with brine
  5. customdried on magnesium sulfate
  6. customthe solvent was removed in a vacuum
  7. customIn this way, 23.5 g (89%) of almost colorless, foamy 5 was obtained
  8. customwhich was used without further purification in the next stage

Quellen und Nachweise

ORD-Eintrag
ord-98a87ce172c440babe195a96c6dbab0f
Quelldatensatz
uspto-grants-2008_05
Patentnummer
US07378404B2

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