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Water → 7-(4-Fluoro-phenyl)-3-iodo-imidazo[1,2-a]pyridine

HRID 341230
ノート
印刷プレビュー

反応式

HRID 341230 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][N:11]3[CH:14]=[CH:15][N:16]=[C:10]3[CH:9]=2)=[CH:4][CH:3]=1.[I:17]N1C(=O)CCC1=O.O>CN(C)C=O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][N:11]3[C:14]([I:17])=[CH:15][N:16]=[C:10]3[CH:9]=2)=[CH:6][CH: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

5

反応物 3

HCID 962WaterHCID 120273N-IodosuccinimideHCID 593207997-(4-Fluoro-phenyl)-imidazo[1,2-a]pyridine

生成物 1

HCID 593207767-(4-Fluoro-phenyl)-3-iodo-imidazo[1,2-a]pyridine収率 29%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 7-(4-fluoro-phenyl)-imidazo[1,2-a]pyridine (13.0 g, 61.3 mmol) in N,N-dimethylformamide (100 mL) stirring under a nitrogen atmosphere at ambient was added N-iodosuccinimide (14.5 g, 64.4 mmol). The reaction mixture was stirred for 2 h and then poured into water (1 L) and stirred for a further 30 min. The solid obtained was collected by filtration, washed with water and air dried on the filter. The solid was triturated with ether, collected by filtration and dried under vacuum at 50° C. The solid obtained was partitioned between water and EtOAc. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure. The solid thus obtained was partitioned between aqueous sodium thiosulphate solution and EtOAc. The organic layer was washed with brine, dried (MgSO4) and concentrated under reduced pressure. The product was triturated with EtOAc, collected by filtration and air-dried to afford 6.0 g (29%) of the title compound. 1H NMR (400 MHz, CDCl3) δ 8.23 (1H, d), 7.91 (1H, s), 7.78 (1H, s), 7.67 (2H, dd), 7.28 (1H, d), 7.22 (2H, t). A further crop of product (11.0 g) containing minor impurities was obtained by evaporating the filtrates under reduced pressure, triturating with petrol/EtOAc and collection by filtration.

後処理

  1. stirringstirred for a further 30 min
  2. customThe solid obtained
  3. filtrationwas collected by filtration
  4. washwashed with water and air
  5. customdried on the filter
  6. customThe solid was triturated with ether
  7. filtrationcollected by filtration
  8. customdried under vacuum at 50° C
  9. customThe solid obtained
  10. customwas partitioned between water and EtOAc
  11. washThe organic layer was washed with brine
  12. dry with materialdried (MgSO4)
  13. filtrationfiltered
  14. concentrationconcentrated under reduced pressure
  15. customThe solid thus obtained
  16. customwas partitioned between aqueous sodium thiosulphate solution and EtOAc
  17. washThe organic layer was washed with brine
  18. dry with materialdried (MgSO4)
  19. concentrationconcentrated under reduced pressure
  20. customThe product was triturated with EtOAc
  21. filtrationcollected by filtration
  22. customair-dried

出典と根拠

ORDレコード
ord-28ddd69c586946899a8a3707ac18036e
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895745B2

反応ノート

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