Sodium Carbonate → Hexafluorophosphate

HRID 1759290ノート

反応式

HRID 1759290 の反応式
[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]

参加物

8

反応物 4

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

生成物 2

HCID 9886HexafluorophosphateHCID 23371075HCID 23371075、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-e623fa1a02a74d7f963d4caab15ac53b
出典データセット
uspto-grants-1982_07
特許番号
US04339567

反応ノート

読み込み中…