Lead tetraacetate → HCID 178419342, 화합물

HRID 40478

반응식

HRID 40478 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 178419342HCID 178419342, 화합물

시약·촉매·용매 2

HCID 15337Mercuric acetate촉매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7a0a3d5313034f89b09bb452f512b217
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530388B2

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