Water → HCID 178507322、化合物

HRID 1843628

反応式

HRID 1843628 の反応式
C([NH:5][C:6]1[CH:11]=[C:10]([C:12]2[C:13]([C:26]3[CH:27]=[C:28]([NH:32][C:33]([NH:35][C:36]4[CH:41]=[CH:40][C:39]([C:42]([F:45])([F:44])[F:43])=[CH:38][CH:37]=4)=[O:34])[CH:29]=[CH:30][CH:31]=3)=[N:14][N:15](CC3C=CC(OC)=CC=3)[CH:16]=2)[CH:9]=[CH:8][N:7]=1)(C)(C)C.O.C([O-])(O)=O.[Na+]>FC(F)(F)C(O)=O>[NH2:5][C:6]1[CH:11]=[C:10]([C:12]2[C:13]([C:26]3[CH:27]=[C:28]([NH:32][C:33]([NH:35][C:36]4[CH:41]=[CH:40][C:39]([C:42]([F:44])([F:45])[F:43])=[CH:38][CH:37]=4)=[O:34])[CH:29]=[CH:30][CH:31]=3)=[N:14][NH:15][CH:16]=2)[CH:9]=[CH:8][N:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 671847851-(3-{4-[2-(tert-butylamino)pyridin-4-yl]-1-(4-methoxybenzyl)-1H-pyrazol-3-yl}phenyl)-3-[4-(trifluoromethyl)phenyl]urea

生成物 1

HCID 178507322HCID 178507322、化合物収率 71.3%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
70 °C

実験手順

100 mg (0.16 mmol) of 1-(3-{4-[2-(tert-butylamino)pyridin-4-yl]-1-(4-methoxybenzyl)-1H-pyrazol-3-yl}phenyl)-3-[4-(trifluoromethyl)phenyl]urea were dissolved in 5 ml of trifluoroacetic acid and the mixture heated at 70° C. under stirring. After 16 hours the solution was poured into icy water, neutralized with aqueous NaHCO3 and extracted with dichloromethane. The organic layer was then dried over Na2SO4 and evaporated to dryness. The product was purified by chromatography on a silica gel column eluted with dichloromethane-methanol (gradient from 1% to 5%) obtaining 50 mg (71% yield) of the title compound.

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic layer was then dried over Na2SO4
  3. customevaporated to dryness
  4. customThe product was purified by chromatography on a silica gel column
  5. washeluted with dichloromethane-methanol (gradient from 1% to 5%)

出典と根拠

ORDレコード
ord-ee5202dba79e47eda546db30d27ca7b7
出典データセット
uspto-grants-2015_02
特許番号
US08946250B2

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