Lead carbonate (PbCO3) → (4-Tert-butoxyphenyl)diphenylsulfonium butanesulfonate

HRID 1418093노트

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HRID 1418093 반응식
[Cl-].[C:2]([O:6][C:7]1[CH:12]=[CH:11][C:10]([S+:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:9][CH:8]=1)([CH3:5])([CH3:4])[CH3:3].C(=O)([O-])[O-].[Pb+2].[CH2:31]([S:35]([OH:38])(=[O:37])=[O:36])[CH2:32][CH2:33][CH3:34]>CO>[CH2:31]([S:35]([O-:38])(=[O:37])=[O:36])[CH2:32][CH2:33][CH3:34].[C:2]([O:6][C:7]1[CH:12]=[CH:11][C:10]([S+:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)=[CH:9][CH:8]=1)([CH3:5])([CH3:3])[CH3:4]

참가 물질

5

반응물 3

HCID 11727Lead carbonate (PbCO3)HCID 499351-Butanesulfonic acidHCID 23435201(4-tert-Butoxyphenyl)(diphenyl)sulfanium chloride

생성물 1

HCID 86753865(4-Tert-butoxyphenyl)diphenylsulfonium butanesulfonate수율 82.3%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
40 °C

실험 절차

In 36 g of methanol was dissolved 3.3 g (0.009 mol) of (4-tert-butoxyphenyl)diphenylsulfonium chloride. 1.7 g (0.0063 mol) of lead carbonate and 1.4 g (0.010 mol) of butanesulfonic acid were added to the solution, which was heated at 40° C. After cooling, the precipitate was filtered off and the filtrate was evaporated. 100 g of chloroform was added to the residue, the solution was washed with 100 g of water, and the solvent layer was evaporated again, obtaining 3.5 g (two-steps yield 64%) of (4-tert-butoxyphenyl)diphenylsulfonium butanesulfonate with 97% purity.

후처리

  1. temperatureAfter cooling
  2. filtrationthe precipitate was filtered off
  3. customthe filtrate was evaporated
  4. addition100 g of chloroform was added to the residue
  5. washthe solution was washed with 100 g of water
  6. customthe solvent layer was evaporated again

출처 및 근거

ORD 기록
ord-a936fab247f842e8bd58006f69df25c3
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05880169

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