3-(1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5,5-dimethyl-2-isoxazoline → HCID 178427280, 화합물

HRID 1172065노트

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HRID 1172065 반응식
C([N:5]1[C:9]([Cl:10])=[C:8]([CH2:11][S:12][C:13]2[CH2:17][C:16]([CH3:19])([CH3:18])[O:15][N:14]=2)[C:7]([C:20]([F:23])([F:22])[F:21])=[N:6]1)(C)(C)C.Br.C(O)(=O)C>O>[Cl:10][C:9]1[NH:5][N:6]=[C:7]([C:20]([F:21])([F:23])[F:22])[C:8]=1[CH2:11][S:12][C:13]1[CH2:17][C:16]([CH3:19])([CH3:18])[O:15][N:14]=1

참가 물질

4

반응물 2

HCID 178628593-(1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5,5-dimethyl-2-isoxazolineHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

생성물 1

HCID 178427280HCID 178427280, 화합물수율 71.6%

시약·촉매·용매 1

HCID 962Water용매

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온도
45 °C

실험 절차

19.8 g (53.4 mmoles) of 3-(1-tert-butyl-5-chloro-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5,5-dimethyl-2-isoxazoline was added to 170 ml of a 25% hydrogen bromide-acetic acid solution. The mixture was stirred at 40 to 50° C. for 2 hours to give rise to a reaction. After the completion of the reaction was confirmed, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and 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 12.0 g (yield: 60.6%) of 3-(5-chloro-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5,5-dimethyl-2-isoxazoline as light yellow crystals (melting point: 120.0 to 122.0° C.).

후처리

  1. customto give rise
  2. customto a reaction
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe resulting organic layer was washed with water
  5. dry with materialan aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to vacuum distillation
  7. customto remove the solvent

출처 및 근거

ORD 기록
ord-34bf047967b34187a1f6662c3e818df5
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07833939B2

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