反応式
[Mn]([O-])(=O)(=O)=O.[K+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[N:14]1[C:18]([C:19]2[O:20]C=CC=2)=[CH:17][C:16]([C:24]([F:27])([F:26])[F:25])=[N:15]1.CC(C)=[O:30].[OH-].[Na+]>O>[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[N:14]1[C:18]([C:19]([OH:20])=[O:30])=[CH:17][C:16]([C:24]([F:27])([F:26])[F:25])=[N:15]1参加物
実験手順
An aqueous solution of 27.94 g of potassium permanganate in 100 ml of water was added dropwise to a mixture of 18.43 g of 1-(2-chlorophenyl)-5-(2-furyl)-3-trifluoromethyl-1H-pyrazole and 250 ml of acetone with being kept at 40° C. or lower. Then, the mixture was stirred at room temperature for 20 hours. The reaction mixture was filtered through Celite (registered trademark) to obtain a filtrate. The filtrate was adjusted to pH 10-12 by an addition of a 2N aqueous sodium hydroxide solution, and then extracted with ethyl acetate two times. The aqueous layer was adjusted to around pH 3 by an addition of 2 N hydrochloric acid, and then extracted with methyl tert-butyl ether three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over magnesium sulfate, and concentrated under reduced pressure to obtain 10.65 g of 1-(2-chlorophenyl)-3-trifluoromethyl-1H-pyrazole-5-carboxylic acid of the formula:
後処理
- customwith being kept at 40° C.
- filtrationThe reaction mixture was filtered through Celite (registered trademark)
- customto obtain a filtrate
- extractionextracted with ethyl acetate two times
- additionThe aqueous layer was adjusted to around pH 3 by an addition of 2 N hydrochloric acid
- extractionextracted with methyl tert-butyl ether three times
- washwashed with an aqueous saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-e7cb78fb2a8c4b68be55749e10866632
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07867949B2
関連ノート
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