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Hydrochloric Acid → N-[3-Fluoro-6-(6-fluoro-1H-indol-4-yl)-1H-indazol-4-yl]-2-methyl-1,3-thiazole-4-carboxamide

HRID 244751
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HRID 244751 반응식
[CH3:1][C:2]1[S:3][CH:4]=[C:5]([C:7]([OH:9])=O)[N:6]=1.ClC(N(C)C)=C(C)C.[F:18][C:19]1[C:27]2[C:26]([NH2:28])=[CH:25][C:24]([C:29]3[CH:37]=[C:36]([F:38])[CH:35]=[C:34]4[C:30]=3[CH:31]=[CH:32][N:33]4S(C3C=CC([N+]([O-])=O)=CC=3)(=O)=O)=[CH:23][C:22]=2[N:21](S(C2C=CC=CC=2)(=O)=O)[N:20]=1.N1C=CC=CC=1.[OH-].[Na+].Cl>C1COCC1.C(O)(C)C.CS(C)=O>[F:18][C:19]1[C:27]2[C:22](=[CH:23][C:24]([C:29]3[CH:37]=[C:36]([F:38])[CH:35]=[C:34]4[C:30]=3[CH:31]=[CH:32][NH:33]4)=[CH:25][C:26]=2[NH:28][C:7]([C:5]2[N:6]=[C:2]([CH3:1])[S:3][CH:4]=2)=[O:9])[NH:21][N:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 6

HCID 313Hydrochloric AcidHCID 1049Pyridine3회HCID 14798Sodium Hydroxide2회HCID 2847282-Methyl-1,3-thiazole-4-carboxylic acid3회HCID 6407921-Chloro-N,N-2-trimethylpropenylamine3회HCID 583564523-Fluoro-6-{6-fluoro-1-[(4-nitrophenyl)sulfonyl]-1H-indol-4-yl}-1-(phenylsulfonyl)-1H-indazol-4-amine

생성물 1

HCID 178433038N-[3-Fluoro-6-(6-fluoro-1H-indol-4-yl)-1H-indazol-4-yl]-2-methyl-1,3-thiazole-4-carboxamide

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 3776Isopropanol용매HCID 8028Tetrahydrofuran용매4회

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온도
80 °C

실험 절차

2-Methyl-1,3-thiazole-4-carboxylic acid was dissolved in THF (0.2 ml) and (1-chloro-2-methyl-1-propen-1-yl)dimethylamine (0.013 ml, 0.1 mmol) was added. The mixture was shaken, then left to stand for 30 mins. 3-fluoro-6-{6-fluoro-1-[(4-nitrophenyl)sulfonyl]-1H-indol-4-yl}-1-(phenylsulfonyl)-1H-indazol-4-amine (0.1 mmol) was dissolved in THF (0.4 ml) and added to the reaction mixture, followed by pyridine (0.016 ml, 0.2 mmol). The reaction mixture was shaken and then left to stand for 1 hour. A further portion of 2-methyl-1,3-thiazole-4-carboxylic acid was dissolved in THF (0.2 ml) and (1-chloro-2-methyl-1-propen-1-yl)dimethylamine (0.013 ml, 0.1 mmol) was added. The mixture was shaken, then left to stand for 20 mins before being added to the ongoing reaction mixture above, along with further pyridine (0.097 ml, 1.2 mmol). The mixture was shaken and left to stand for 30 mins. A further portion of 2-methyl-1,3-thiazole-4-carboxylic acid was dissolved in THF (0.2 ml) and (1-chloro-2-methyl-1-propen-1-yl)dimethylamine (0.013 ml, 0.1 mmol) was added. The mixture was shaken, then left to stand for 20 mins before being added to the ongoing reaction mixture above, along with further pyridine (0.097 ml, 1.2 mmol). The mixture was shaken and left to stand for 30 mins, then evaporated by blow down under a stream of nitrogen. The crude reaction mixture was dissolved in isopropanol (0.3 ml) and NaOH (2M aqueous, 0.3 ml) was added. The mixture was stood for 60 h at room temperature. Further NaOH (2M aqueous, 0.3 ml) was added and the mixture was heated to 80° C. for 1 hour. The reaction mixture was neutralised with HCl (2 M, aq.) and blown down under a stream of nitrogen. The crude material was dissolved in DMSO (0.5 ml), filtered and purified by Mass Directed Auto Prep on an Xbridge column using Acetonitrile/Water with a formic acid modifier (Method F). The solvent was evaporated in vacuo using the Genevac. The residue was dissolved in DMSO (0.5 ml) and further purified by formic acid MDAP (as above), over an extended run time. The product-containing fractions were blown down under a stream of nitrogen to give the title compound (11 mg). LCMS (Method D) Rt=1.16 min, MH+=410.

후처리

  1. waitleft
  2. additionadded to the reaction mixture
  3. stirringThe reaction mixture was shaken
  4. waitleft
  5. waitto stand for 1 hour
  6. stirringThe mixture was shaken
  7. waitleft
  8. waitto stand for 20 mins
  9. stirringThe mixture was shaken
  10. waitleft
  11. waitto stand for 30 mins
  12. stirringThe mixture was shaken
  13. waitleft
  14. waitto stand for 20 mins
  15. stirringThe mixture was shaken
  16. waitleft
  17. waitto stand for 30 mins
  18. customevaporated by blow down under a stream of nitrogen
  19. customThe crude reaction mixture
  20. waitThe mixture was stood for 60 h at room temperature
  21. filtrationfiltered
  22. custompurified by Mass Directed Auto Prep on an Xbridge column
  23. customThe solvent was evaporated in vacuo
  24. dissolutionThe residue was dissolved in DMSO (0.5 ml)
  25. customfurther purified by formic acid MDAP (as above), over an extended run time

출처 및 근거

ORD 기록
ord-b7b94bf04cef4030afdb1b280fe18065
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658635B2

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