Potassium Carbonate → HCID 178476524、化合物

HRID 1191562ノート

反応式

HRID 1191562 の反応式
[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

参加物

4

反応物 3

HCID 11430Potassium CarbonateHCID 45097455(5-Bromo-2-methylphenyl)boronic acidHCID 178418268HCID 178418268、化合物

生成物 1

HCID 178476524HCID 178476524、化合物収率 78.9%

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3815df7ca815481aa0e8040fdf2f7242
出典データセット
uspto-grants-2014_03
特許番号
US08680012B2

反応ノート

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