Potassium Carbonate → HCID 178476524, 화합물

HRID 1470870

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HRID 1470870 반응식
[C:1]([O-:4])(=[O:3])[CH3:2].[C:5]([O-:8])(=[O:7])[CH3:6].[C:9]([O-:12])(=[O:11])[CH3:10].C([O-])(=O)C.[Pb+4:17].[Br:18][C:19]1[CH:20]=[CH:21][C:22]([CH3:28])=[C:23](B(O)O)[CH:24]=1.C(=O)([O-])[O-].[K+].[K+]>>[C:1]([O-:4])(=[O:3])[CH3:2].[C:5]([O-:8])(=[O:7])[CH3:6].[C:9]([O-:12])(=[O:11])[CH3:10].[Br:18][C:19]1[CH:20]=[CH:21][C:22]([CH3:28])=[C:23]([Pb+3:17])[CH:24]=1

참가 물질

4

반응물 3

HCID 11430Potassium CarbonateHCID 45097455(5-Bromo-2-methylphenyl)boronic acidHCID 178418268HCID 178418268, 화합물

생성물 1

HCID 178476524HCID 178476524, 화합물수율 78.9%

반응 조건

온도
40 °C

실험 절차

To a mixture of lead tetraacetate (11.25 g, 25.40 mmol) and mercuric diacetate (0.40 g, 1.27 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (35 ml). This mixture is warmed to 40° C., and 5-bromo-2-methylphenylboronic acid (4.96 g, 23.10 mmol) is added in one portion and the suspension is heated at this temperature for 5 hours. The mixture is then allowed to cool to room temperature, followed by further cooling to 0° C. then powdered anhydrous potassium carbonate (1.61 g) is added with rapid stirring for 5 minutes. The mixture is filtered, the filtrate is concentrated to half its volume, and hexanes added to induce precipitation. This mixture is further concentrated, the solvent decanted, and the solid washed with hexanes to afford 5-bromo-2-methylphenyllead triacetate (10.10 g) as a sandy coloured solid.

후처리

  1. customthoroughly flushed with nitrogen
  2. additionis added anhydrous chloroform (35 ml)
  3. temperaturethe suspension is heated at this temperature for 5 hours
  4. temperatureto cool to room temperature
  5. temperatureby further cooling to 0° C.
  6. additionis added
  7. filtrationThe mixture is filtered
  8. concentrationthe filtrate is concentrated to half its volume, and hexanes
  9. additionadded
  10. customprecipitation
  11. customthe solvent decanted
  12. washthe solid washed with hexanes

출처 및 근거

ORD 기록
ord-104c256fdf884c679016ce1544b2a2dd
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006429B2

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