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

HRID 1172065ノート

反応式

HRID 1172065 の反応式
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

参加物

4

反応物 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

生成物 1

HCID 178427280HCID 178427280、化合物収率 71.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
45 °C

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-34bf047967b34187a1f6662c3e818df5
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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