5-{2-[6-Methyl-4-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-thiazol-4-yl}-thiophene-2-sulfonic acid tert-butylamide → 5-{2-[6-Methyl-4-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-thiazol-4-yl}-thiophene-2-sulfonic acid amide

HRID 1989633ノート

反応式

HRID 1989633 の反応式
C([NH:5][S:6]([C:9]1[S:10][C:11]([C:14]2[N:15]=[C:16]([C:19]3[CH:24]=[C:23]([C:25]4[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][CH:26]=4)[CH:22]=[C:21]([CH3:35])[N:20]=3)[S:17][CH:18]=2)=[CH:12][CH:13]=1)(=[O:8])=[O:7])(C)(C)C>C(O)(C(F)(F)F)=O>[CH3:35][C:21]1[N:20]=[C:19]([C:16]2[S:17][CH:18]=[C:14]([C:11]3[S:10][C:9]([S:6]([NH2:5])(=[O:8])=[O:7])=[CH:13][CH:12]=3)[N:15]=2)[CH:24]=[C:23]([C:25]2[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:32])[F:33])=[CH:27][CH:26]=2)[CH:22]=1

参加物

3

反応物 1

HCID 247598725-{2-[6-Methyl-4-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-thiazol-4-yl}-thiophene-2-sulfonic acid tert-butylamide

生成物 1

HCID 574690445-{2-[6-Methyl-4-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-thiazol-4-yl}-thiophene-2-sulfonic acid amide収率 83.7%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
23 °C

実験手順

To 5-{2-[6-methyl-4-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-thiazol-4-yl}-thiophene-2-sulfonic acid tert-butylamide (example 324) (0.100 g, 0.186 mmol) was added TFA (10 mL) and the reaction mixture was stirred at 23° C. for 16 h. The mixture was evaporated to dryness and partitioned between EtOAc and saturated NaHCO3 solution, the organic layer was dried over Na2SO4. Removal of the solvent in vacuum left a crude product which was triturated with diethyl ether to give the title compound as a white solid (0.075 g, 83%). MS (ISP) 482.3 [(M+H)+].

後処理

  1. customThe mixture was evaporated to dryness
  2. custompartitioned between EtOAc and saturated NaHCO3 solution
  3. dry with materialthe organic layer was dried over Na2SO4
  4. customRemoval of the solvent in vacuum
  5. waitleft a crude product which
  6. customwas triturated with diethyl ether

出典と根拠

ORDレコード
ord-ef272687f4184d0cad2ca1b26b286174
出典データセット
uspto-grants-2010_01
特許番号
US07642264B2

反応ノート

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