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Trifluoromethanesulfonic acid → 7-(2-Aminopyrimidin-5-yl)-1-{[(1r)-1-cyclopropyl-2,2,2-trifluoroethyl]amino}-8-iodo-5h-pyrido[4,3-b]indole-4-carboxamide

HRID 1971026
ノート
印刷プレビュー

反応式

HRID 1971026 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[C:12]4[C:20]([NH:21][C@H:22]([CH:27]5[CH2:29][CH2:28]5)[C:23]([F:26])([F:25])[F:24])=[N:19][CH:18]=[C:17]([C:30]([NH2:32])=[O:31])[C:13]=4[NH:14][C:15]=3[CH:16]=2)=[CH:4][N:3]=1.[B-](F)(F)(F)F.C1C=CN=CC=1.C1C=CN=CC=1.[IH2+:50].FC(F)(F)S(O)(=O)=O.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[NH2:1][C:2]1[N:3]=[CH:4][C:5]([C:8]2[C:9]([I:50])=[CH:10][C:11]3[C:12]4[C:20]([NH:21][C@H:22]([CH:27]5[CH2:29][CH2:28]5)[C:23]([F:25])([F:24])[F:26])=[N:19][CH:18]=[C:17]([C:30]([NH2:32])=[O:31])[C:13]=4[NH:14][C:15]=3[CH:16]=2)=[CH:6][N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 62406Trifluoromethanesulfonic acid2 回HCID 516892Sodium BicarbonateHCID 10883201Bis(pyridine)iodonium tetrafluoroborate2 回HCID 426229347-(2-Aminopyrimidin-5-yl)-1-{[(1r)-1-cyclopropyl-2,2,2-trifluoroethyl]amino}-5h-pyrido[4,3-b]indole-4-carboxamide

生成物 1

HCID 42636082
7-(2-Aminopyrimidin-5-yl)-1-{[(1r)-1-cyclopropyl-2,2,2-trifluoroethyl]amino}-8-iodo-5h-pyrido[4,3-b]indole-4-carboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred slurry of 7-(2-aminopyrimidin-5-yl)-1-{[(1R)-1-cyclopropyl-2,2,2-trifluoroethyl]amino}-5H-pyrido[4,3-b]indole-4-carboxamide (60 mg, 0.14 mmol) and bis(pyridine)iodonium tetrafluoroborate (152 mg, 0.41 mmol) in DCM (2.5 mL) was added trifluoromethanesulfonic acid (0.11 mL, 1.2 mmol). The reaction mixture was left to stir for 2 d, treated with additional bis(pyridine)iodonium tetrafluoroborate (152 mg, 0.41 mmol) and trifluoromethanesulfonic acid (0.07 mL, 0.8 mmol), and left to stir for 6 h. The mixture was diluted with DCM and treated with sodium bicarbonate solution. The mixture was extracted with EtOAc, and the combined organics were washed with brine, dried (sodium sulfate), concentrated, and purified by flash chromatography to afford the title compound. 1H NMR (600 MHz, CD3SOCD3) δ 11.78 (s, 1H); 9.02 (s, 1H), 8.51 (s, 1H); 8.23 (s, 2H); 7.92 (br s, 1H); 7.70 (s, 1H); 7.78 (br s, 1H); 7.77 (d, 1H); 6.80 (s, 2H); 4.87 (m, 1H); 1.58 (m, 1H); 0.73 (m, 1H); 0.62 (m, 1H); 0.54 (m, 1H); 0.32 (m, 1H). LRMS (APCI) calc'd for (C21H17IF3N7O) [M+H]+, 568.0. found 568.0.

後処理

  1. waitThe reaction mixture was left
  2. waitleft
  3. stirringto stir for 6 h
  4. extractionThe mixture was extracted with EtOAc
  5. washthe combined organics were washed with brine
  6. dry with materialdried (sodium sulfate)
  7. concentrationconcentrated
  8. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-8aac347ff4004cb6885173fd9474f421
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08431569B2

反応ノート

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