Methanesulfenyl chloride, trifluoro- → HCID 22591644, 화합물

HRID 22866노트

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HRID 22866 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:17]([NH:18][CH2:19][C:20]2[CH:25]=[N:24][CH:23]=[CH:22][N:21]=2)=[CH:16][CH:15]=[N:14]1.[F:26][C:27]([F:31])([F:30])[S:28]Cl.C(=O)([O-])O.[Na+]>C(Cl)Cl>[Cl:12][C:4]1[CH:5]=[C:6]([C:8]([F:9])([F:10])[F:11])[CH:7]=[C:2]([Cl:1])[C:3]=1[N:13]1[C:17]([NH:18][CH2:19][C:20]2[CH:25]=[N:24][CH:23]=[CH:22][N:21]=2)=[C:16]([S:28][C:27]([F:31])([F:30])[F:26])[CH:15]=[N:14]1

참가 물질

5

반응물 3

HCID 67900Methanesulfenyl chloride, trifluoro-HCID 516892Sodium BicarbonateHCID 22591646HCID 22591646, 화합물

생성물 1

HCID 22591644HCID 22591644, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 3.0 g of 1-(2,6-dichloro-4-trifluoromethylphenyl)-5-(pyrazin-2-ylmethylamino)pyrazole dissolved in 30 ml of dried methylene chloride under a nitrogen atmosphere was added 14 ml of dried methylene chloride solution of trifluoromethylsulfenyl chloride at room temperature over about 1 hour, followed by stirring overnight. Saturated aqueous sodium hydrogen carbonate solution was added thereto, and the organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and water several times. Thereafter, the layer was purified by a silica gel column chromatography. After removal of solvent, drying in vacuo afforded 3.59 g of 1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfenyl-5-(pyrazin-2-ylmethylamino)pyrazole.

후처리

  1. washthe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and water several times
  2. customThereafter, the layer was purified by a silica gel column chromatography
  3. customAfter removal of solvent
  4. customdrying in vacuo

출처 및 근거

ORD 기록
ord-bd89ebcad29448aa87d9d887ef9be4bb
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849633B2

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