Water → 5,5-dimethyl-3-(5-ethylthio-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline

HRID 1292763ノート

反応式

HRID 1292763 の反応式
[OH-].[Na+].O.[CH2:4]([SH:6])[CH3:5].[CH3:7][C:8]1([CH3:31])[O:12][N:11]=[C:10]([S:13][CH2:14][C:15]2[C:16]([C:27]([F:30])([F:29])[F:28])=[N:17][N:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:19]=2F)[CH2:9]1>CN(C)C=O>[CH3:7][C:8]1([CH3:31])[O:12][N:11]=[C:10]([S:13][CH2:14][C:15]2[C:16]([C:27]([F:30])([F:29])[F:28])=[N:17][N:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:19]=2[S:6][CH2:4][CH3:5])[CH2:9]1

参加物

6

反応物 4

HCID 962Water2 回HCID 6343EthanethiolHCID 14798Sodium HydroxideHCID 178628915,5-dimethyl-3-(5-fluoro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline

生成物 1

HCID 178628935,5-dimethyl-3-(5-ethylthio-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline収率 103.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

0.2 g (4.0 mmoles) of sodium hydroxide and 1 ml of water were added to a solution of 0.25 g (4.0 mmoles) of ethanethiol dissolved in 10 ml of N,N-dimethylformamide. The mixture was stirred at room temperature for 30 minutes. Thereto was added a solution of 0.5 g (1.4 mmoles) of 5,5-dimethyl-3-(5-fluoro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline dissolved in 5 ml of N,N-dimethylformamide. The resulting mixture was stirred 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 ethyl acetate. 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 0.6 g (yield: 100%) of 5,5-dimethyl-3-(5-ethylthio-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-2-isoxazoline.

後処理

  1. stirringThe resulting mixture was stirred for 1 hour
  2. customto give rise
  3. customto a reaction
  4. customAfter the completion of the reaction
  5. extractionfollowed by extraction with ethyl acetate
  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

出典と根拠

ORDレコード
ord-044a275280c4470194003db9392647bc
出典データセット
uspto-grants-2007_07
特許番号
US07238689B2

反応ノート

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