Trifluoroacetic acid → HCID 178486747, 화합물

HRID 228957

반응식

HRID 228957 반응식
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][NH:23][C:24]([NH:33]C(OC(C)(C)C)=O)=[N:25]C(OC(C)(C)C)=O)[N:16]=[CH:15][CH:14]=[C:13]2[O:41][C:42]1[C:43]([CH3:52])=[N:44][C:45]2[C:50]([CH:51]=1)=[CH:49][CH:48]=[CH:47][CH:46]=2.[OH-].[Na+]>>[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][NH:23][C:24]([NH2:33])=[NH:25])[N:16]=[CH:15][CH:14]=[C:13]2[O:41][C:42]1[C:43]([CH3:52])=[N:44][C:45]2[C:50]([CH:51]=1)=[CH:49][CH:48]=[CH:47][CH:46]=2

참가 물질

4

반응물 3

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 178486746HCID 178486746, 화합물

생성물 1

HCID 178486747HCID 178486747, 화합물수율 100%

반응 조건

온도
0 °C

실험 절차

Trifluoroacetic acid (1 ml) was added to N-{2-[6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-7-yloxy]-ethyl}-N′,N″-diboc-guanidine (222 mg) at 0° C., and the mixture was then stirred at 0° C. for 2 hr. The reaction solution was made alkaline by the addition of a 1 N aqueous sodium hydroxide solution and was extracted with n-butanol. The n-butanol layer was washed with water and was then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (150 mg, yield 100%).

후처리

  1. extractionwas extracted with n-butanol
  2. washThe n-butanol layer was washed with water
  3. dry with materialwas then dried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customthe residue was purified by thin layer chromatography

출처 및 근거

ORD 기록
ord-1473569bef484c709de4853e270842aa
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560558B2

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