Lead tetraacetate → HCID 178419342，化合物

HRID 40478

反应方程式

HRID 40478 反应方程式
[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

参与物

6

反应物 3

HCID 11025Lead tetraacetateHCID 11430碳酸钾HCID 58061455(5-Bromo-2-cyclopropylphenyl)boronic acid

产物 1

HCID 178419342HCID 178419342，化合物

试剂、催化剂与溶剂 2

HCID 15337乙酸汞催化剂HCID 6212三氯甲烷溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-7a0a3d5313034f89b09bb452f512b217
来源数据集
uspto-grants-2013_09
专利号
US08530388B2

关联笔记

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