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Ethanol → 4-(9H-pyrido[2,3-b]indol-6-yl)thiazol-2(3H)-one

HRID 341281
ノート
印刷プレビュー

反応式

HRID 341281 の反応式
[S-:1][C:2]#[N:3].[K+].Br[CH2:6][C:7]([C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[NH:14][C:13]1[N:18]=[CH:19][CH:20]=[CH:21][C:12]2=1)=O.C([OH:24])C>>[N:18]1[C:13]2[NH:14][C:15]3[C:11]([C:12]=2[CH:21]=[CH:20][CH:19]=1)=[CH:10][C:9]([C:7]1[NH:3][C:2](=[O:24])[S:1][CH:6]=1)=[CH:17][CH:16]=3
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 702Ethanol2 回HCID 516872Potassium thiocyanateHCID 585145292-bromo-1-(9H-pyrido[2,3-b]indol-6-yl)ethanone

生成物 1

HCID 585145014-(9H-pyrido[2,3-b]indol-6-yl)thiazol-2(3H)-one

実験手順

A solution of potassium thiocyanate (73 mg, 0.73 mmol, 2 equiv.) in Ethanol (1 mL), was added dropwise a solution of compound 2-Bromo-1-(9H-pyrido[2,3-b]indol-6-yl)ethanone (150 mg, 0.366 mmol) in ethanol (1 mL). The mixture was stirred at reflux for 1 hour. The resulting mixture was then cautiously quenched at 0° C. with H2O. It was extracted with EtOAc. The resulting organic layer was washed with NaCl saturated aqueous solution, dried over MgSO4, and filtered. Solvent was removed under reduced pressure The crude product was triturated and filtered. The resulting product (82 mg, 0276 mmol) was dissolved in glacial acetic acid (1 mL), 50% sulfuric acid (200 μL) was added, and then the mixture was heated to reflux for 1 hour. The resulting mixture was quenched at 0° C. with H2O. The aqueous layer is treated with Na2CO3 until pH=6 and then extracted with AcOEt (3×20 ml). The organic layers was washed with NaCl saturated aqueous solution, dried over MgSO4, and filtered. Solvent was removed under reduced pressure. A white powder was obtained in 23% yield after trituration of the crude product in MeOH and filtration; 1H NMR (300 MHz, DMSO-d6): δ 11.96 (bs, 1H), 11.78 (bs, 1H), 8.48-8.43 (m, 3H), 7.74 (dd, 1H, J=1.9, 8.5 Hz), 7.52 (d, 1H, J=8.5 Hz), 7.25 (dd, 1H, J=5.5, 7.2 Hz), 6.69 (d, 1H, J=1.9 Hz), 4.75 (bs, 1H); MS (ESI) m/z 268.1 [M+H+]

後処理

  1. temperatureat reflux for 1 hour
  2. customThe resulting mixture was then cautiously quenched at 0° C. with H2O
  3. extractionIt was extracted with EtOAc
  4. washThe resulting organic layer was washed with NaCl saturated aqueous solution
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customSolvent was removed under reduced pressure The crude product
  8. customwas triturated
  9. filtrationfiltered
  10. dissolutionThe resulting product (82 mg, 0276 mmol) was dissolved in glacial acetic acid (1 mL)
  11. addition50% sulfuric acid (200 μL) was added
  12. temperaturethe mixture was heated
  13. temperatureto reflux for 1 hour
  14. customThe resulting mixture was quenched at 0° C. with H2O
  15. additionThe aqueous layer is treated with Na2CO3 until pH=6
  16. extractionextracted with AcOEt (3×20 ml)
  17. washThe organic layers was washed with NaCl saturated aqueous solution
  18. dry with materialdried over MgSO4
  19. filtrationfiltered
  20. customSolvent was removed under reduced pressure
  21. customA white powder was obtained in 23% yield
  22. filtrationafter trituration of the crude product in MeOH and filtration

出典と根拠

ORDレコード
ord-701fd2885c0543a99a44ae31d976e655
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895744B2

反応ノート

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