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1,4-Dioxane → 1-(1-Methylethyl)-N-[6-(2-methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-indazol-4-yl]-1H-pyrazole-5-carboxamide

HRID 244741
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HRID 244741 반응식
Br[C:2]1[CH:3]=[C:4]([NH:17][C:18]([C:20]2[N:24]([CH:25]([CH3:27])[CH3:26])[N:23]=[CH:22][CH:21]=2)=[O:19])[C:5]2[C:9]([CH:10]=1)=[N:8][N:7](C1CCCCO1)[CH:6]=2.[CH3:28][C:29]1[NH:40][C:32]2=[N:33][CH:34]=[CH:35][C:36](B(O)O)=[C:31]2[CH:30]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].O1CCOCC1>CO.O>[CH3:27][CH:25]([N:24]1[C:20]([C:18]([NH:17][C:4]2[CH:3]=[C:2]([C:36]3[CH:35]=[CH:34][N:33]=[C:32]4[NH:40][C:29]([CH3:28])=[CH:30][C:31]=34)[CH:10]=[C:9]3[C:5]=2[CH:6]=[N:7][NH:8]3)=[O:19])=[CH:21][CH:22]=[N:23]1)[CH3:26]
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참가 물질

7

반응물 4

HCID 312751,4-DioxaneHCID 62657Potassium Phosphate, Tribasic2회HCID 58255796N-[6-Bromo-2-(tetrahydro-2H-pyran-2-yl)-2H-indazol-4-yl]-1-(1-methylethyl)-1H-pyrazole-5-carboxamideHCID 59744427(2-Methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)boronic acid3회

생성물 1

HCID 583563711-(1-Methylethyl)-N-[6-(2-methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-indazol-4-yl]-1H-pyrazole-5-carboxamide

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

A microwave vial was charged with N-[6-bromo-2-(tetrahydro-2H-pyran-2-yl)-2H-indazol-4-yl]-1-(1-methylethyl)-1H-pyrazole-5-carboxamide (70 mg), (2-methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)boronic acid (29 mg), tripotassium phosphate (103 mg) and Solvias catalyst (9 mg), 1,4-dioxane (1.2 ml) and water (0.24 ml). The reaction was heated under microwave irradiation at 100° C. for 30 min, twice. Further (2-methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)boronic acid (10 mg) and Solvias catalyst (9 mg) were added and the reaction heated under microwave irradiation at 100° C. for 30 min. Again further (2-methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)boronic acid (11 mg), tripotassium phosphate (30 mg) and Solvias catalyst (9 mg) were added and the reaction heated under microwave irradiation at 100° C. for 30 min. The reaction was passed through a silica cartridge, preconditioned with methanol, washing with methanol. The solvent was evaporated and the residue was dissolved in DMSO:methanol (1:1, v/v) and purified by MDAP (Method A). Appropriate fractions were evaporated to dryness, dissolved in methanol (2 ml) and 2 M HCl (aq) (0.5 ml) and left at room temperature for 30 min. The solvent was evaporated, the residue was dissolved in DMSO:methanol (1:10, v/v) and passed through an aminopropyl cartridge preconditioned with methanol, washing with methanol. The solvent was evaporated and the residue was purified by MDAP (method A). Purified fractions were evaporated to dryness, dissolved in methanol, passed through an aminopropyl cartridge preconditioned with methanol, washing with methanol, then evaporated to dryness to give title compound, 19 mg.

후처리

  1. temperaturethe reaction heated under microwave irradiation at 100° C. for 30 min
  2. temperaturethe reaction heated under microwave irradiation at 100° C. for 30 min
  3. washwashing with methanol
  4. customThe solvent was evaporated
  5. dissolutionthe residue was dissolved in DMSO:methanol (1:1
  6. customv/v) and purified by MDAP (Method A)
  7. customAppropriate fractions were evaporated to dryness
  8. dissolutiondissolved in methanol (2 ml)
  9. customThe solvent was evaporated
  10. dissolutionthe residue was dissolved in DMSO:methanol (1:10
  11. washwashing with methanol
  12. customThe solvent was evaporated
  13. customthe residue was purified by MDAP (method A)
  14. customPurified fractions were evaporated to dryness
  15. dissolutiondissolved in methanol
  16. washwashing with methanol
  17. customevaporated to dryness

출처 및 근거

ORD 기록
ord-af660087b4ce4a07b8844f3471b80964
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658635B2

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