N-Iodosuccinimide → 2-(2,4-difluorophenyl)-3-iodo-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole

HRID 1930029ノート

反応式

HRID 1930029 の反応式
C1C(=O)N([I:8])C(=O)C1.[F:9][C:10]1[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:11]=1[C:17]1[N:18]=[C:19]2[CH2:24][CH2:23][CH2:22][N:20]2[CH:21]=1>CN(C=O)C>[F:9][C:10]1[CH:15]=[C:14]([F:16])[CH:13]=[CH:12][C:11]=1[C:17]1[N:18]=[C:19]2[CH2:24][CH2:23][CH2:22][N:20]2[C:21]=1[I:8]

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 579298552-(2,4-difluorophenyl)-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole

生成物 1

HCID 579298822-(2,4-difluorophenyl)-3-iodo-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole収率 43.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

NIS (6.75 g, 30.0 mmol) was added to a solution of 2-(2,4-difluorophenyl)-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole (6.61 g, 30.0 mmol) in DMF (50 mL). The reaction mixture was stirred at ambient temperature for about 35 min and then partitioned between DCM and water. The organics were dried over MgSO4, filtered, concentrated under reduced pressure, and triturated with Et2O to give the title compound (4.49 g, 43%): LC/MS (Table 1, Method a) Rt=3.18 min; MS m/z: 347.2 (M+H)+.

後処理

  1. custompartitioned between DCM and water
  2. dry with materialThe organics were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customtriturated with Et2O

出典と根拠

ORDレコード
ord-590de5093728471db82ab5570749c8cd
出典データセット
uspto-grants-2012_05
特許番号
US08188083B2

反応ノート

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