Water → 5-Bromomethyl-4-ethoxy-6-trifluoromethylpyrimidine

HRID 254221ノート

反応式

HRID 254221 の反応式
[CH2:1]([O:3][C:4]1[C:9]([CH2:10]O)=[C:8]([C:12]([F:15])([F:14])[F:13])[N:7]=[CH:6][N:5]=1)[CH3:2].P(Br)(Br)[Br:17].O>CCOCC.CO>[Br:17][CH2:10][C:9]1[C:4]([O:3][CH2:1][CH3:2])=[N:5][CH:6]=[N:7][C:8]=1[C:12]([F:15])([F:14])[F:13]

参加物

6

反応物 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 17862901(4-Ethoxy-6-trifluoromethylpyrimidin-5-yl)-methanol

生成物 1

HCID 178628575-Bromomethyl-4-ethoxy-6-trifluoromethylpyrimidine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of 3.77 g (17.0 mmoles) of (4-ethoxy-6-trifluoromethylpyrimidin-5-yl)-methanol dissolved in 50 ml of ether was cooled to 0° C. Thereto was added 2.0 g (7.2 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature for 1 hour. The resulting salt was dissolved in methanol and the solution was stirred for 1 hour to give rise to a reaction. The reaction mixture was poured into water and extraction with ether was conducted. 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 reduced pressure distillation to remove the solvent contained therein, to obtain a crude product of 5-bromomethyl-4-ethoxy-6-trifluoromethylpyrimidine.

後処理

  1. stirringthe solution was stirred for 1 hour
  2. customto give rise
  3. customto a reaction
  4. washThe resulting organic layer was washed with an aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to reduced pressure distillation
  7. customto remove the solvent

出典と根拠

ORDレコード
ord-175b5ee55b8e4b03915ba128de3ac962
出典データセット
uspto-grants-2011_01
特許番号
US07875606B2

反応ノート

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