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

HRID 1172134ノート

反応式

HRID 1172134 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].CO.O>C(OCC)C>[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 4

HCID 887MethanolHCID 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 1

HCID 3283Diethyl Ether溶媒

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 diethyl 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 using methanol. The resulting mixture was stirred for 1 hour to give rise to a 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 crude 5-bromomethyl-4-ethoxy-6-trifluoromethylpyrimidine.

後処理

  1. dissolutionThe resulting salt was dissolved
  2. stirringThe resulting mixture was stirred for 1 hour
  3. customto give rise
  4. customto a reaction
  5. extractionfollowed by extraction with diethyl ether
  6. washThe resulting organic layer was washed with an aqueous sodium chloride solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe resulting solution was subjected to vacuum distillation
  9. customto remove the solvent

出典と根拠

ORDレコード
ord-2f419be3589441148fa331254a205b4d
出典データセット
uspto-grants-2010_11
特許番号
US07833939B2

反応ノート

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