5,5-dimethyl-3-(3-methoxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline → 5,5-dimethyl-3-(3-hydroxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline

HRID 1172070노트

반응식

HRID 1172070 반응식
C(O)(=O)C.Br.[CH3:6][C:7]1([CH3:26])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([O:24]C)=[N:16][N:17]([CH3:23])[C:18]=2[C:19]([F:22])([F:21])[F:20])[CH2:8]1>>[CH3:6][C:7]1([CH3:26])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([OH:24])=[N:16][N:17]([CH3:23])[C:18]=2[C:19]([F:22])([F:21])[F:20])[CH2:8]1

참가 물질

3

반응물 2

HCID 178628515,5-dimethyl-3-(3-methoxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazolineHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

생성물 1

HCID 1784819505,5-dimethyl-3-(3-hydroxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline수율 96%

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온도
50 °C

실험 절차

To 20 ml of a 25% hydrogen bromide acetic acid solution was added 3.3 g (10.6 mmoles) of 5,5-dimethyl-3-(3-methoxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline. The mixture was stirred at 50° C. for 3 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was subjected to vacuum distillation to remove the solvent contained therein. The residue was poured into water. The resulting crystals were collected by filtration, washed with water and dried to obtain 3.1 g (yield: 96.0%) of intended 5,5-dimethyl-3-(3-hydroxy-1-methyl-5-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline.

후처리

  1. customto give rise
  2. customto a reaction
  3. customAfter the completion of the reaction
  4. distillationthe reaction mixture was subjected to vacuum distillation
  5. customto remove the solvent
  6. additionThe residue was poured into water
  7. filtrationThe resulting crystals were collected by filtration
  8. washwashed with water
  9. customdried

출처 및 근거

ORD 기록
ord-699948a3dbe240c4afddbc07931d26f5
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07833939B2

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