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

HRID 254221노트

반응식

HRID 254221 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 3283Diethyl Ether용매2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-175b5ee55b8e4b03915ba128de3ac962
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875606B2

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