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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
ノート
印刷プレビュー

反応式

HRID 244741 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 312751,4-DioxaneHCID 62657Potassium Phosphate, Tribasic2 回HCID 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 acid3 回

生成物 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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af660087b4ce4a07b8844f3471b80964
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658635B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート