Sodium Carbonate → Hexafluorophosphate

HRID 1759290Notes

Reaction equation

[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]

Participants

Conditions

Temperature: 20 °C

Procedure

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.

Workup

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

Sources & evidence

ORD record: ord-e623fa1a02a74d7f963d4caab15ac53b
Source dataset: uspto-grants-1982_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04339567

Reaction notes

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