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Water → 5-Bromo-4-chloro-6-(trifluoromethyl)pyrimidine

HRID 254218
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HRID 254218 반응식
[Br:1][C:2]1[C:3](O)=[N:4][CH:5]=[N:6][C:7]=1[C:8]([F:11])([F:10])[F:9].P(Cl)(Cl)([Cl:15])=O.O>C(Cl)(Cl)Cl>[Br:1][C:2]1[C:3]([Cl:15])=[N:4][CH:5]=[N:6][C:7]=1[C:8]([F:11])([F:10])[F:9]
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참가 물질

5

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 178518144CID 11299507

생성물 1

HCID 115362505-Bromo-4-chloro-6-(trifluoromethyl)pyrimidine수율 82.4%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
100 °C

실험 절차

24.3 g (100.0 mmoles) of 5-bromo-4-hydroxy-6-trifluoromethylpyrimidine was suspended in 18.5 g (120.0 mmoles) of phosphorus oxychloride. The suspension was stirred at 100° C. for 2 hours to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was gradually poured into water and extraction with chloroform was conducted. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein. The residue was purified by silica gel column chromatography to obtain 21.5 g (yield: 82.4%) of 5-bromo-4-chloro-6-trifluoromethylpyrimidine.

후처리

  1. customto give rise
  2. customto a reaction
  3. customAfter confirmation of the completion of the reaction
  4. washThe resulting organic layer was washed with water
  5. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to reduced pressure distillation
  7. customto remove the solvent
  8. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-1571258e7a394e5997e2b14e2e997dad
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07875606B2

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