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Sodium Carbonate → 5-[4-(2-Methylsulfanyl-pyrimidin-4-yl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazol-3-yl]-1H-pyrrolo[2,3-b]pyridine

HRID 500738
ノート
印刷プレビュー

反応式

HRID 500738 の反応式
I[C:2]1[C:6]([C:7]2[CH:12]=[CH:11][N:10]=[C:9]([S:13][CH3:14])[N:8]=2)=[CH:5][N:4]([CH:15]2[CH2:20][CH2:19][CH2:18][CH2:17][O:16]2)[N:3]=1.CC1(C)C(C)(C)OB([C:29]2[CH:30]=[C:31]3[CH:37]=[CH:36][NH:35][C:32]3=[N:33][CH:34]=2)O1.C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C>[CH3:14][S:13][C:9]1[N:8]=[C:7]([C:6]2[C:2]([C:29]3[CH:30]=[C:31]4[CH:37]=[CH:36][NH:35][C:32]4=[N:33][CH:34]=3)=[N:3][N:4]([CH:15]3[CH2:20][CH2:19][CH2:18][CH2:17][O:16]3)[CH:5]=2)[CH:12]=[CH:11][N:10]=1
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

5

反応物 3

HCID 10340Sodium Carbonate2 回HCID 242087895-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrrolo(2,3-b)pyridineHCID 594244104-(3-Iodo-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl)-2-(methylthio)pyrimidine

生成物 1

HCID 578562535-[4-(2-Methylsulfanyl-pyrimidin-4-yl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazol-3-yl]-1H-pyrrolo[2,3-b]pyridine収率 69%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
85 °C

実験手順

To a solution of 4-[3-Iodo-1-(tetrahydro-pyran-2-yl)-1H-pyrazol-4-yl]-2-methylsulfanyl-pyrimidine B (1.33 g, 3.3 mmol) and 5-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)-1H-pyrrolo[2,3-b]pyridine (1 g, 4.1 mmol) in DMF (30 mL) was added a 2M solution of sodium carbonate (2 mL). The sodium carbonate appeared to come out of solution upon addition. The mixture was deoxygenated with a nitrogen bubbler for a few minutes. The palladium catalyst was added and nitrogen bubbling continued for a few minutes before the bubbler was removed. The mixture was heated at 85° C. for 18 hr. LCMS shows complete conversion to product. The mixture was dropped into saturated aqueous NaCl and the resulting solids collected by filtration and rinsed with water. The solids were dissolved in methanol/dichloromethane (1:9), dried over MgSO4 and reduced to minimum volume. The residue was purified on a short column of silica gel using a gradient of 0-50% ethyl acetate in dichloromethane as eluant to give 5-[4-(2-Methylsulfanyl-pyrimidin-4-yl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazol-3-yl]-1H-pyrrolo[2,3-b]pyridine (C-1-1) (0.89 g, 69%) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 11.73 (br. s., 1H), 8.69 (s, 1H), 8.43 (d, J=5.31 Hz, 1H), 8.29 (d, J=2.02 Hz, 1H), 8.07 (d, J=2.02 Hz, 1H), 7.51 (t, J=3.03 Hz, 1H), 7.11 (d, J=5.31 Hz, 1H), 6.48 (dd, J=3.28, 1.77 Hz, 1H), 5.53 (dd, J=9.85, 2.27 Hz, 1H), 4.00 (br. d, J=13.39 Hz, 1H), 3.61-3.76 (br. m, 1H), 2.10-2.24 (br. m, 4H), 1.91-2.06 (br. m, 2H), 1.65-1.80 (br. m, 1H), 1.50-1.63 (br. m, 2H).

後処理

  1. additionto come out of solution upon addition
  2. customThe mixture was deoxygenated with a nitrogen bubbler for a few minutes
  3. additionThe palladium catalyst was added
  4. waitnitrogen bubbling continued for a few minutes before the bubbler
  5. customwas removed
  6. additionThe mixture was dropped into saturated aqueous NaCl
  7. filtrationthe resulting solids collected by filtration
  8. washrinsed with water
  9. dissolutionThe solids were dissolved in methanol/dichloromethane (1:9)
  10. dry with materialdried over MgSO4
  11. customThe residue was purified on a short column of silica gel using a gradient of 0-50% ethyl acetate in dichloromethane as eluant

出典と根拠

ORDレコード
ord-2e1d19e9b8e145689de26a3bba3ca2dd
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07772246B2

反応ノート

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