Water → HCID 136109406, 화합물

HRID 429253

반응식

HRID 429253 반응식
[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]

참가 물질

8

반응물 4

HCID 962WaterHCID 3352FipronilHCID 8471Triethylamine2회HCID 443297Hydroxyamine hydrochloride2회

생성물 1

HCID 136109406HCID 136109406, 화합물수율 65.5%

시약·촉매·용매 3

HCID 8058Hexane용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-7478df3361dc4c8b894a280c733d45fc
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06316477B1

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