Water → HCID 178507322, 화합물

HRID 45840

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HRID 45840 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.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

참가 물질

5

반응물 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

생성물 1

HCID 178507322HCID 178507322, 화합물수율 71.3%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

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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 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.

후처리

  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%)

출처 및 근거

ORD 기록
ord-2382139c37fe4b77b98fccfef3125b6f
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541575B2

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