Lead tetraacetate → HCID 178419342、化合物

HRID 40478

反応式

HRID 40478 の反応式
[CH3:1][C:2]([O-:4])=[O:3].[CH3:5][C:6]([O-:8])=[O:7].[CH3:9][C:10]([O-:12])=[O:11].CC([O-])=O.[Pb+2:17].[Br:18][C:19]1[CH:20]=[CH:21][C:22]([CH:28]2[CH2:30][CH2:29]2)=[C:23](B(O)O)[CH:24]=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl.C([O-])(=O)C.[Hg+2].C([O-])(=O)C>[C:2]([O-:4])(=[O:3])[CH3:1].[C:6]([O-:8])(=[O:7])[CH3:5].[C:10]([O-:12])(=[O:11])[CH3:9].[Br:18][C:19]1[CH:20]=[CH:21][C:22]([CH:28]2[CH2:30][CH2:29]2)=[C:23]([Pb+3:17])[CH:24]=1

参加物

6

反応物 3

HCID 11025Lead tetraacetateHCID 11430Potassium CarbonateHCID 58061455(5-Bromo-2-cyclopropylphenyl)boronic acid

生成物 1

HCID 178419342HCID 178419342、化合物

試薬・触媒・溶媒 2

HCID 15337Mercuric acetate触媒HCID 6212Chloroform溶媒

実験手順

To a solution of lead(IV)acetate (4.0 g, 0.0089 mol) and mercury(II)acetate (139 mg, 0.45 mmol) in chloroform (12 ml) at 50° C. is added 5-bromo-2-cyclopropylphenyl boronic acid (2.0 g, 0.0083 mol), and the solution is heated at this temperature for 5 hours. After cooling to room temperature the suspension is further cooled to 0° C. and anhydrous potassium carbonate (1.8 g) is added with rapid stirring for 2 minutes. The reaction mixture is then filtered (washing with additional chloroform), and the filtrate is concentrated to half its original volume and the crude product is precipitated with hexanes. Further concentration then filtration affords 5-bromo-2-cyclopropylphenyl lead triacetate as a beige solid.

後処理

  1. temperaturethe solution is heated at this temperature for 5 hours
  2. temperatureis further cooled to 0° C.
  3. filtrationThe reaction mixture is then filtered
  4. wash(washing with additional chloroform)
  5. concentrationthe filtrate is concentrated to half its original volume
  6. customthe crude product is precipitated with hexanes
  7. concentrationFurther concentration
  8. filtrationfiltration

出典と根拠

ORDレコード
ord-7a0a3d5313034f89b09bb452f512b217
出典データセット
uspto-grants-2013_09
特許番号
US08530388B2

関連ノート

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