Lead carbonate (PbCO3) → Tris(4-tert-butoxyphenyl)sulfonium butanesulfonate

HRID 1418091ノート

反応式

HRID 1418091 の反応式
[Cl-].[C:2]([O:6][C:7]1[CH:12]=[CH:11][C:10]([S+:13]([C:25]2[CH:30]=[CH:29][C:28]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[CH:27][CH:26]=2)[C:14]2[CH:19]=[CH:18][C:17]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:16][CH:15]=2)=[CH:9][CH:8]=1)([CH3:5])([CH3:4])[CH3:3].C(=O)([O-])[O-].[Pb+2].[CH2:41]([S:45]([OH:48])(=[O:47])=[O:46])[CH2:42][CH2:43][CH3:44]>CO>[CH2:41]([S:45]([O-:48])(=[O:47])=[O:46])[CH2:42][CH2:43][CH3:44].[C:21]([O:20][C:17]1[CH:16]=[CH:15][C:14]([S+:13]([C:10]2[CH:11]=[CH:12][C:7]([O:6][C:2]([CH3:5])([CH3:4])[CH3:3])=[CH:8][CH:9]=2)[C:25]2[CH:30]=[CH:29][C:28]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[CH:27][CH:26]=2)=[CH:19][CH:18]=1)([CH3:22])([CH3:23])[CH3:24]

参加物

5

反応物 3

HCID 11727Lead carbonate (PbCO3)HCID 499351-Butanesulfonic acidHCID 85759090Tris(4-tert-butoxyphenyl)sulfonium chloride

生成物 1

HCID 86753864Tris(4-tert-butoxyphenyl)sulfonium butanesulfonate収率 82.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

In 93 g of methanol was dissolved 9.3 g (0.018 mol) of tris(4-tert-butoxyphenyl)sulfonium chloride. 3.5 g (0.013 mol) of lead carbonate and 3.0 g (0.022 mol) of butanesulfonic acid were added to the solution, which was heated at 50 ° C. After cooling, the precipitate was filtered off and the filtrate was evaporated. Then 100 g of chloroform was added to the residue, the solution was washed with 100 g of water, and the solution was evaporated again, obtaining 9.2 g (two-steps yield 29%) of tris(4-tert-butoxyphenyl)sulfonium butanesulfonate with 97% purity.

後処理

  1. temperatureAfter cooling
  2. filtrationthe precipitate was filtered off
  3. customthe filtrate was evaporated
  4. additionThen 100 g of chloroform was added to the residue
  5. washthe solution was washed with 100 g of water
  6. customthe solution was evaporated again

出典と根拠

ORDレコード
ord-ef297e23860f4141874630b2a6c199c1
出典データセット
uspto-grants-1999_03
特許番号
US05880169

反応ノート

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