Trifluoroacetic acid → HCID 178507322, 화합물

HRID 1843648

반응식

HRID 1843648 반응식
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

참가 물질

5

반응물 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

생성물 1

HCID 178507322HCID 178507322, 화합물수율 90%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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%)

출처 및 근거

ORD 기록
ord-e7574ead918c4c0584485cffeb993e17
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946250B2

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