Methanesulfenyl chloride, trifluoro- → HCID 22591644、化合物

HRID 22866

反応式

HRID 22866 の反応式
[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

参加物

5

反応物 3

HCID 67900Methanesulfenyl chloride, trifluoro-HCID 516892Sodium BicarbonateHCID 22591646HCID 22591646、化合物

生成物 1

HCID 22591644HCID 22591644、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bd89ebcad29448aa87d9d887ef9be4bb
出典データセット
uspto-grants-2005_02
特許番号
US06849633B2

関連ノート

読み込み中…