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

HRID 254218
ノート
印刷プレビュー

反応式

HRID 254218 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 178518144CID 11299507

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1571258e7a394e5997e2b14e2e997dad
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07875606B2

反応ノート

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