Water → 4-bromomethyl-5-fluoro-1-phenyl-3-trifluoromethyl-1H-pyrazole

HRID 1292791ノート

反応式

HRID 1292791 の反応式
[F:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([C:13]([F:16])([F:15])[F:14])[C:3]=1[CH2:17]O.P(Br)(Br)[Br:20].O>C(OCC)C>[Br:20][CH2:17][C:3]1[C:4]([C:13]([F:16])([F:15])[F:14])=[N:5][N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:2]=1[F:1]

参加物

5

反応物 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 17862906(5-fluoro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol

生成物 1

HCID 178629274-bromomethyl-5-fluoro-1-phenyl-3-trifluoromethyl-1H-pyrazole収率 253.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

A solution of 27.5 g (105.7 mmoles) of (5-fluoro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol dissolved in 300 ml of diethyl ether was cooled to 0° C. Thereto was added 10.0 g (37.0 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature for 2 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into water, followed by extraction with diethyl ether. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein, to obtain 30.3 g (yield: 88.8%) of 4-bromomethyl-5-fluoro-1-phenyl-3-trifluoromethyl-1H-pyrazole.

後処理

  1. customto give rise
  2. customto a reaction
  3. customAfter the completion of the reaction
  4. extractionfollowed by extraction with diethyl ether
  5. washThe resulting organic layer was washed with an aqueous sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe resulting solution was subjected to vacuum distillation
  8. customto remove the solvent

出典と根拠

ORDレコード
ord-df0ee044718a4688ad80bc2a37448b5c
出典データセット
uspto-grants-2007_07
特許番号
US07238689B2

反応ノート

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