4-Bromo-2-ethylphenylboronic acid → HCID 178476529、化合物

HRID 341698

反応式

HRID 341698 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:24]=[CH:23][C:22](B(O)O)=[C:21]([CH2:28][CH3:29])[CH:20]=1>>[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:24]=[CH:23][C:22]([Pb+3:17])=[C:21]([CH2:28][CH3:29])[CH:20]=1

参加物

3

反応物 2

HCID 592760174-Bromo-2-ethylphenylboronic acidHCID 178418268HCID 178418268、化合物

生成物 1

HCID 178476529HCID 178476529、化合物収率 44.8%

反応条件

温度
40 °C

実験手順

To a mixture of lead tetraacetate (53 g, 0.12 mol) and mercuric diacetate (2.5 g, 0.0078 mol), thoroughly flushed with nitrogen, is added anhydrous chloroform (250 ml). This mixture is warmed to 40° C. and 4-bromo-2-ethylphenylboronic acid (25 g, 0.11 mol) is added in one portion and the mixture is stirred and heated at this temperature for 4 hours. After cooling to room temperature, cooled in an ice bath, filtered through a plug of diatomaceous earth and the filtrate is concentrated to approximately a quarter of its volume. Hexane is added to induce crystallization and the solvents evaporated under reduced pressure. Trituration with hexane gives 4-bromo-2-ethylphenyl lead triacetate (28 g).

後処理

  1. customthoroughly flushed with nitrogen
  2. additionis added anhydrous chloroform (250 ml)
  3. temperatureheated at this temperature for 4 hours
  4. temperatureAfter cooling to room temperature
  5. temperaturecooled in an ice bath
  6. filtrationfiltered through a plug of diatomaceous earth
  7. concentrationthe filtrate is concentrated to approximately a quarter of its volume
  8. additionHexane is added
  9. customcrystallization
  10. customthe solvents evaporated under reduced pressure

出典と根拠

ORDレコード
ord-66c96b4989b54d7cac56c093b825e16e
出典データセット
uspto-grants-2014_11
特許番号
US08895761B2

関連ノート

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