Sodium Carbonate → Hexafluorophosphate

HRID 1759290노트

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HRID 1759290 반응식
[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]

참가 물질

8

반응물 4

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

생성물 2

HCID 9886HexafluorophosphateHCID 23371075HCID 23371075, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

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온도
20 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e623fa1a02a74d7f963d4caab15ac53b
출처 데이터셋
uspto-grants-1982_07
특허 번호
US04339567

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