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Potassium Carbonate → [Diacetyloxy-(5-bromo-2-chlorophenyl)plumbyl] acetate

HRID 72272
ノート
印刷プレビュー

反応式

HRID 72272 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]([Cl: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]([Cl:28])=[C:23]([Pb+3:17])[CH:24]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 11430Potassium CarbonateHCID 467368165-Bromo-2-chlorophenylboronic acidHCID 178418268HCID 178418268、化合物

生成物 1

HCID 178476543[Diacetyloxy-(5-bromo-2-chlorophenyl)plumbyl] acetate収率 91.8%

反応条件

温度
40 °C

実験手順

To a mixture of lead tetraacetate (26.83 g, 61 mmol) and mercuric diacetate (0.77 g, 2.4 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (50 ml) and the reaction mixture is stirred and heated to 40° C. 5-Bromo-2-chlorophenylboronic acid (11.39 g, 48 mmol) is added in one portion, and the reaction mixture is stirred at 40° C. for 4 hours. After cooling to room temperature potassium carbonate (3.34 g) is added, the mixture stirred vigorously for 5 minutes and then filtered. The filtrate is concentrated in vacuo to give 5-bromo-2-chlorophenyllead triacetate (25.33 g), used without further purification in the next step.

後処理

  1. customthoroughly flushed with nitrogen
  2. additionis added anhydrous chloroform (50 ml)
  3. stirringthe reaction mixture is stirred at 40° C. for 4 hours
  4. additionis added
  5. stirringthe mixture stirred vigorously for 5 minutes
  6. filtrationfiltered
  7. concentrationThe filtrate is concentrated in vacuo

出典と根拠

ORDレコード
ord-5918d1ad95c54bb393b00a1f81bdb61d
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08828908B2

反応ノート

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