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 1172070ノート

反応式

HRID 1172070 の反応式
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

参加物

3

反応物 2

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

生成物 1

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

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-699948a3dbe240c4afddbc07931d26f5
出典データセット
uspto-grants-2010_11
特許番号
US07833939B2

反応ノート

読み込み中…