Sodium Carbonate → Hexafluorophosphate

HRID 1759290Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1759290
[F:1][P-:2]([F:7])([F:6])([F:5])([F:4])[F:3].[C:8]1([S+:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(=O)([O-])[O-:28].[Na+].[Na+].ClC1C=C(C=CC=1)C(OO)=O.S([O-])([O-])(=O)=S.[Na+].[Na+]>O.CC(C)=O>[F:1][P-:2]([F:7])([F:6])([F:5])([F:4])[F:3].[C:21]1([S+:14]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:28])[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1.[F:1][P-:2]([F:7])([F:6])([F:5])([F:4])[F:3]

Komponenten

8

Edukt 4

HCID 10340Sodium CarbonateHCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 93819Sulfonium, triphenyl-, hexafluorophosphate(1-) (1:1)

Produkt 2

HCID 9886HexafluorophosphateHCID 23371075HCID 23371075, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

A mixture consisting of 157 parts of acetone, 4 parts of triphenylsulphonium hexafluorophosphate, 8.48 parts of sodium carbonate, and 17.2 parts of m-chloroperoxybenzoic acid was stirred at 20° C. for 24 hours. A solution of 40 parts of sodium thiosulphate in 500 parts of water was added. The acetone was removed under reduced pressure and triphenylsulphoxonium hexafluorophosphate was filtered off and dried under vacuum at 50° C. The desired product thus obtained (V1, R7 =H, R6 =C6H4, p=zero, R8 =R9 =C6H5, r=1, Zr- =PF6-), had m.pt. 233°-238° C., NMR (acetone-d6) 7.8-8.3 (m); I.R. (KBr disc) 3100, 3070, 1450, 1225, 1080, 840, 760, 730, 685 cm-1 ; UV (ethanol) λmax 232 nm and 270 nm.

Aufarbeitung

  1. customThe acetone was removed under reduced pressure and triphenylsulphoxonium hexafluorophosphate
  2. filtrationwas filtered off
  3. customdried under vacuum at 50° C

Quellen und Nachweise

ORD-Eintrag
ord-e623fa1a02a74d7f963d4caab15ac53b
Quelldatensatz
uspto-grants-1982_07
Patentnummer
US04339567

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