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Bromine → 2-Bromo-2-[2-(methylthio-4-pyrimidinyl)]-1-phenylethanone

HRID 2212869
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HRID 2212869 반응식
[Br:1]Br.[CH3:3][S:4][C:5]1[N:10]=[C:9]([CH2:11][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:13])[CH:8]=[CH:7][N:6]=1>C(O)(=O)C>[Br:1][CH:11]([C:9]1[CH:8]=[CH:7][N:6]=[C:5]([S:4][CH3:3])[N:10]=1)[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24408Bromine3회HCID 129858292-[2-(Methylsulfanyl)pyrimidin-4-yl]-1-phenylethan-1-one

생성물 1

HCID 129858302-Bromo-2-[2-(methylthio-4-pyrimidinyl)]-1-phenylethanone

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Bromine (24.1 g, 0.15 mol) is added with stirring to 2-(2-methylthio-pyrimidin-4-yl)-1-phenyl-ethanone (36.8 g, 0.15 mol) in acetic acid (300 ml) in such a way that the reaction temperature does not exceed +25° C. and the color of the bromine is discharged immediately. After the addition of the bromine solution the solvent is removed by evaporation under vacuum. The pH of the resulting oil is adjusted to 8 using an aqueous saturated sodium bicarbonate solution and the product is extracted several times with diethylther. Drying the combined extracts with magnesium sulfate, filtering and evaporation of the solvent gives the crude 2-bromo-2-(2-methylthio-pyrimidin-4-yl)-1-phenyl-ethanone in form of an oil of sufficient purity for the following step.

후처리

  1. customdoes not exceed +25° C.
  2. customis removed by evaporation under vacuum
  3. extractionthe product is extracted several times with diethylther
  4. dry with materialDrying the combined extracts with magnesium sulfate
  5. filtrationfiltering
  6. customevaporation of the solvent

출처 및 근거

ORD 기록
ord-7247a1ba44ba47bda4393e8b1fbc9a89
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07105517B2

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