Trifluoroacetic acid → 3-[6-Methyl-4-(4-trifluoromethyl-phenyl)-[2,3']bipyridinyl-5'-yl]-benzenesulfonamide

HRID 1989602ノート

反応式

HRID 1989602 の反応式
C([NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]2[CH:16]=[C:17]([C:21]3[CH:26]=[C:25]([C:27]4[CH:32]=[CH:31][C:30]([C:33]([F:36])([F:35])[F:34])=[CH:29][CH:28]=4)[CH:24]=[C:23]([CH3:37])[N:22]=3)[CH:18]=[N:19][CH:20]=2)[CH:10]=1)(=[O:8])=[O:7])(C)(C)C.C(O)(C(F)(F)F)=O>ClCCl>[CH3:37][C:23]1[N:22]=[C:21]([C:17]2[CH:18]=[N:19][CH:20]=[C:15]([C:11]3[CH:10]=[C:9]([S:6]([NH2:5])(=[O:8])=[O:7])[CH:14]=[CH:13][CH:12]=3)[CH:16]=2)[CH:26]=[C:25]([C:27]2[CH:32]=[CH:31][C:30]([C:33]([F:36])([F:34])[F:35])=[CH:29][CH:28]=2)[CH:24]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 24760815N-tert-Butyl-3-[6-methyl-4-(4-trifluoromethyl-phenyl)-[2,3']bipyridinyl-5'-yl]-benzenesulfonamide

生成物 1

HCID 247608913-[6-Methyl-4-(4-trifluoromethyl-phenyl)-[2,3']bipyridinyl-5'-yl]-benzenesulfonamide収率 97%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred and cooled suspension of N-tert-butyl-3-[6-methyl-4-(4-trifluoromethylphenyl)-[2,3′]bipyridinyl-5′-yl]-benzenesulfonamide (example 288) (0.150 g, 0.29 mmol) in dichloromethane (0.9 mL) was added TFA (6.3 mL) and the reaction mixture was allowed to stir at room temperature for 16 h. The mixture was evaporated to dryness and saturated NaHCO3 solution (5 mL), diethyl ether and heptane were added. The mixture was stirred at room temperature for 1 h, the precipitate was collected by filtration, washed with water and heptane/diethyl ether and dried to yield the title compound as a white solid (0.130 g, 97%). MS (ISP) 470.3 [(M+H)+]; mp 235° C. (dec.).

後処理

  1. temperaturecooled
  2. stirringto stir at room temperature for 16 h
  3. customThe mixture was evaporated to dryness and saturated NaHCO3 solution (5 mL), diethyl ether and heptane
  4. additionwere added
  5. stirringThe mixture was stirred at room temperature for 1 h
  6. filtrationthe precipitate was collected by filtration
  7. washwashed with water and heptane/diethyl ether
  8. customdried

出典と根拠

ORDレコード
ord-cd9bd1b3f9864f58905c5588c01e0135
出典データセット
uspto-grants-2010_01
特許番号
US07642264B2

反応ノート

読み込み中…