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

HRID 1930029노트

반응식

HRID 1930029 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-590de5093728471db82ab5570749c8cd
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188083B2

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