(5-Chloro-2-methylphenyl)boronic acid → [Diacetyloxy-(5-chloro-2-methylphenyl)plumbyl] acetate

HRID 72256

반응식

HRID 72256 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].[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([CH3:28])=[C:23](B(O)O)[CH:24]=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].[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([CH3:28])=[C:23]([Pb+3:17])[CH:24]=1

참가 물질

3

반응물 2

HCID 2773336(5-Chloro-2-methylphenyl)boronic acidHCID 178418268HCID 178418268, 화합물

생성물 1

HCID 178476526[Diacetyloxy-(5-chloro-2-methylphenyl)plumbyl] acetate수율 99.8%

반응 조건

온도
40 °C

실험 절차

To a mixture of lead tetraacetate (2.15 g, 4.85 mmol) and mercuric diacetate (0.15 g, 0.47 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (6 ml). This mixture is warmed to 40° C., and 5-chloro-2-methylphenylboronic acid (0.76 g, 4.46 mmol) is added in one portion, and the suspension is heated at this temperature for 5 hours. After cooling to room temperature the mixture is concentrated to a small volume then triturated with hexanes and filtered to yield crude 5-chloro-2-methylphenyllead triacetate (2.27 g).

후처리

  1. customthoroughly flushed with nitrogen
  2. additionis added anhydrous chloroform (6 ml)
  3. temperaturethe suspension is heated at this temperature for 5 hours
  4. temperatureAfter cooling to room temperature the mixture
  5. concentrationis concentrated to a small volume
  6. customthen triturated with hexanes
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-f409628f8ca04feda77bcdf7b29091e2
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08828908B2

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