Phosphorus pentachloride → HCID 14878964, Verbindung

HRID 2371471Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2371471
O[CH2:2][C:3]([CH3:21])([CH3:20])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:23]>C1(C)C(C)=CC=CC=1>[Cl:23][CH2:2][C:3]([CH3:21])([CH3:20])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]=1

Komponenten

4

Edukt 2

HCID 24819Phosphorus pentachlorideHCID 13854275HCID 13854275, Verbindung

Produkt 1

HCID 14878964HCID 14878964, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

0.5 Gram of 6-phenoxy-2-pyridylmethyl 3-hydroxy-2,2-dimethylpropyl ether was dissolved in 20 ml of dry xylene, and 0.73 g of phosphorus pentachloride was added, followed by heating under reflux for 3 hours. Thereafter, the reaction solution was poured into ice water and extracted with xylene. The xylene layer was washed with water, dried and concentrated. The residue was subjected to column chromatography on silica gel (developing solvent, hexane:ethyl acetate=50:1) to obtain 90 mg of desired 6-phenoxy-2-pyridylmethyl 3-chloro-2,2-dimethylpropyl ether [present compound (1)].

Aufarbeitung

  1. temperatureby heating
  2. temperatureunder reflux for 3 hours
  3. extractionextracted with xylene
  4. washThe xylene layer was washed with water
  5. customdried
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-12ba5b14d02d4dca82ef757dfdaa25db
Quelldatensatz
uspto-grants-1992_03
Patentnummer
US05093373

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