Trifluoroacetic acid → HCID 178507322、化合物

HRID 1843648

反応式

HRID 1843648 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.FC(F)(F)C(O)=O.[Na]>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 6422Trifluoroacetic acidHCID 5360545SodiumHCID 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 90%

試薬・触媒・溶媒 1

HCID 962Water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 with 5 ml of trifluoroacetic acid and the solution stirred at 70° C. for 6 hours. The mixture was then poured into icy water, neutralized with aqueous sodium hydrogenocarbonate and extracted with ethylacetate. The organic layer was dried over sodium sulphate and evaporated to dryness. The residue was purified by flash-chromatography on a silica gel column (dichloromethane-methanol, from 1% to 10%), giving 63 mg (90%) of the title compound.

後処理

  1. extractionextracted with ethylacetate
  2. dry with materialThe organic layer was dried over sodium sulphate
  3. customevaporated to dryness
  4. customThe residue was purified by flash-chromatography on a silica gel column (dichloromethane-methanol, from 1% to 10%)

出典と根拠

ORDレコード
ord-e7574ead918c4c0584485cffeb993e17
出典データセット
uspto-grants-2015_02
特許番号
US08946250B2

関連ノート

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