Tetrahydrofuran → N-[2-chloro-6-(hydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-3-trifluoromethyl-1H-pyrazole-5-carboxamide

HRID 251898

반응식

HRID 251898 반응식
[Cl:1][C:2]1[C:11]2[N:10]=[C:9]([C:12]3[N:16]([C:17]4[C:22]([Cl:23])=[CH:21][CH:20]=[CH:19][N:18]=4)[N:15]=[C:14]([C:24]([F:27])([F:26])[F:25])[CH:13]=3)[O:8][C:7](=[O:28])[C:6]=2[CH:5]=[CH:4][CH:3]=1.O.[NH2:30][NH2:31].O1CCCC1>O>[Cl:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]([C:7]([NH:30][NH2:31])=[O:28])[C:11]=1[NH:10][C:9]([C:12]1[N:16]([C:17]2[C:22]([Cl:23])=[CH:21][CH:20]=[CH:19][N:18]=2)[N:15]=[C:14]([C:24]([F:27])([F:26])[F:25])[CH:13]=1)=[O:8]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 24654Hydrazine hydrate (1:1)HCID 574377918-chloro-2-[1-(3-chloro-2-pyridinyl)-3-trifluoromethyl-1H-pyrazol-5-yl]-4H-3,1-benzoxazine-4-one

생성물 1

HCID 66854209N-[2-chloro-6-(hydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-3-trifluoromethyl-1H-pyrazole-5-carboxamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 0.27 g of 8-chloro-2-[1-(3-chloro-2-pyridinyl)-3-trifluoromethyl-1H-pyrazol-5-yl]-4H-3,1-benzoxazine-4-one, 0.025 ml of hydrazine monohydrate and 10 ml of tetrahydrofuran was stirred at room temperature for 3 hours. Water was poured into the reaction mixture, and the mixture was extracted with ethyl acetate three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was washed with a mixed solvent of chloroform and methyl t-butyl ether to obtain 0.21 g of N-[2-chloro-6-(hydrazinocarbonyl)phenyl]-1-(3-chloro-2-pyridinyl)-3-trifluoromethyl-1H-pyrazole-5-carboxamide of the formula:

후처리

  1. extractionthe mixture was extracted with ethyl acetate three times
  2. washwashed with an aqueous saturated sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. washThe resulting residue was washed with a mixed solvent of chloroform and methyl t-butyl ether

출처 및 근거

ORD 기록
ord-30a159e607d14f07967f6d335bcdd979
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07867949B2

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