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

HRID 1470877
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HRID 1470877 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].[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
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참가 물질

4

반응물 3

HCID 11430Potassium CarbonateHCID 467368165-Bromo-2-chlorophenylboronic acidHCID 178418268HCID 178418268, 화합물

생성물 1

HCID 178476543[Diacetyloxy-(5-bromo-2-chlorophenyl)plumbyl] acetate수율 82.3%

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온도
40 °C

실험 절차

To a mixture of lead tetraacetate (1.46 g, 3.3 mmol) and mercuric diacetate (42 mg, 0.13 mmol), thoroughly flushed with nitrogen, is added anhydrous chloroform (2.5 ml) is introduced and the reaction mixture is stirred and heated to 40° C. 5-Bromo-2-chlorophenylboronic acid (0.62 g, 2.6 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 (0.18 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 (1.23 g), used without further purification in the next step.

후처리

  1. customthoroughly flushed with nitrogen
  2. additionis added anhydrous chloroform (2.5 ml)
  3. additionis introduced
  4. stirringthe reaction mixture is stirred at 40° C. for 4 hours
  5. additionis added
  6. stirringthe mixture stirred vigorously for 5 minutes
  7. filtrationfiltered
  8. concentrationThe filtrate is concentrated in vacuo

출처 및 근거

ORD 기록
ord-55f1c3fa5d5044a9853d22391a1914d7
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006429B2

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