Water → HCID 136109406、化合物

HRID 429253

反応式

HRID 429253 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]#[N:20])[C:3]=1[S:21]([C:23]([F:26])([F:25])[F:24])=[O:22].Cl.[NH2:28][OH:29].C(N(CC)CC)C.O>O1CCOCC1.C(OCC)(=O)C.CCCCCC>[NH2:1][C:2]1[N:6]([C:7]2[C:8]([Cl:18])=[CH:9][C:10]([C:14]([F:15])([F:16])[F:17])=[CH:11][C:12]=2[Cl:13])[N:5]=[C:4]([C:19](=[N:28][OH:29])[NH2:20])[C:3]=1[S:21]([C:23]([F:25])([F:24])[F:26])=[O:22]

参加物

8

反応物 4

HCID 962WaterHCID 3352FipronilHCID 8471Triethylamine2 回HCID 443297Hydroxyamine hydrochloride2 回

生成物 1

HCID 136109406HCID 136109406、化合物収率 65.5%

試薬・触媒・溶媒 3

HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

5-Amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfinylpyrazole (500 mg, 1.1 mmol) and hydroxylamine hydrochloride (79 mg, 1.1 mmol) were dissolved in 5 ml of dioxane, and then triethylamine (115 mg, 1.1 mmol) was added at room temperature. After the mixture was stirred at room temperature for 6 hours, hydroxylamine hydrochloride (79 mg, 1.1 mmol) and triethylamine (115 mg, 1.1 mmol) were further added, followed by stirring at room temperature for 2 hours. The reaction mixture was poured into 100 ml of iced water and extracted with 100 ml of ethyl acetate. The extract was dried over anhydrous magnesium sulfate and then concentrated to obtain a brown oily substance. This oily substance was subjected to silica gel column chromatography [eluent: mixed solvent of n-hexane and ethyl acetate (volume ratio=3:1)] to obtain 340 mg (0.72 mmol) of the title compound as a colorless crystal. Yield 63%.

後処理

  1. stirringby stirring at room temperature for 2 hours
  2. extractionextracted with 100 ml of ethyl acetate
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customto obtain a brown oily substance

出典と根拠

ORDレコード
ord-7478df3361dc4c8b894a280c733d45fc
出典データセット
uspto-grants-2001_11
特許番号
US06316477B1

関連ノート

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