Methyl p-toluenesulfonate → Bis(4-tert-butylphenyl)iodonium p-toluenesulfonate

HRID 2057131ノート

反応式

HRID 2057131 の反応式
[Cl-].[C:2]([C:6]1[CH:11]=[CH:10][C:9]([I+:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:15][CH:14]=2)=[CH:8][CH:7]=1)([CH3:5])([CH3:4])[CH3:3].[C:23]1([CH3:34])[CH:28]=[CH:27][C:26]([S:29]([O:32]C)(=[O:31])=[O:30])=[CH:25][CH:24]=1>COC(C)(C)C>[C:23]1([CH3:34])[CH:24]=[CH:25][C:26]([S:29]([O-:32])(=[O:30])=[O:31])=[CH:27][CH:28]=1.[C:19]([C:16]1[CH:17]=[CH:18][C:13]([I+:12][C:9]2[CH:8]=[CH:7][C:6]([C:2]([CH3:5])([CH3:4])[CH3:3])=[CH:11][CH:10]=2)=[CH:14][CH:15]=1)([CH3:22])([CH3:21])[CH3:20]

参加物

4

反応物 2

HCID 6645Methyl p-toluenesulfonateHCID 21889439Iodonium, bis[4-(1,1-dimethylethyl)phenyl]-, chloride

生成物 1

HCID 16216932Bis(4-tert-butylphenyl)iodonium p-toluenesulfonate収率 91%

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

実験手順

Bis(p-tert-butylphenyl)iodonium chloride (428.8 g; 1.0 mol) and methyl p-toluenesulfonate (223.5 g; 1.2 mol) were suspended in t-butyl methyl ether (500 ml). The suspension was heated at 55° C.-58° C. and refluxed for 5 hours while being stirred. After the reaction mixture had been cooled, formed white solid was separated through filtration. The white solid was washed with t-butyl methyl ether and dried under vacuum, to thereby yield 513.7 g of bis(p-tert-butylphenyl)iodonium p-toluenesulfonate (yield: 91%).

後処理

  1. temperatureThe suspension was heated at 55° C.-58° C.
  2. temperaturerefluxed for 5 hours
  3. temperatureAfter the reaction mixture had been cooled
  4. customformed white solid
  5. customwas separated through filtration
  6. washThe white solid was washed with t-butyl methyl ether
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-c7a7c722a05b4f349299c987db3f1bc7
出典データセット
uspto-grants-2008_02
特許番号
US07335787B2

反応ノート

読み込み中…