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Water → 4-Bromomethyl-5-methyl-3-trifluoromethylisoxazole

HRID 1172119
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HRID 1172119 반응식
[CH3:1][C:2]1[O:6][N:5]=[C:4]([C:7]([F:10])([F:9])[F:8])[C:3]=1[CH2:11]O.P(Br)(Br)[Br:14].O>C(OCC)C>[Br:14][CH2:11][C:3]1[C:4]([C:7]([F:10])([F:9])[F:8])=[N:5][O:6][C:2]=1[CH3:1]
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참가 물질

5

반응물 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 17862894(5-Methyl-3-trifluoromethylisoxazol-4-yl)-methanol

생성물 1

HCID 178628854-Bromomethyl-5-methyl-3-trifluoromethylisoxazole수율 82%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of 0.45 g (2.5 mmoles) of (5-methyl-3-trifluoromethylisoxazol-4-yl)-methanol dissolved in 10 ml of diethyl ether was cooed to 0° C. Thereto was added 0.2 g (8.9 mmoles) of phosphorus tribromide. The mixture was stirred at room temperature for 1 hour 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 0.5 g (yield: 74.0%) of 4-bromomethyl-5-methyl-3-trifluoromethylisoxazole.

후처리

  1. customwas cooed to 0° C
  2. customto give rise
  3. customto a reaction
  4. customAfter the completion of the 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

출처 및 근거

ORD 기록
ord-0157d62e35264bd4bbb7bf877828ed18
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07833939B2

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