Water → 5-chloro-7-fluoro-1-methyl-2-pyridin-3-yl-1H-indole

HRID 1661635노트

반응식

HRID 1661635 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([F:11])[CH:10]=1)[NH:7][C:6]([C:12]1[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=1)=[CH:5]2.[H-].[Na+].I[CH3:21].O>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([F:11])[CH:10]=1)[N:7]([CH3:21])[C:6]([C:12]1[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=1)=[CH:5]2

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 595346575-chloro-7-fluoro-2-pyridin-3-yl-1H-indole

생성물 1

HCID 582155765-chloro-7-fluoro-1-methyl-2-pyridin-3-yl-1H-indole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5-chloro-7-fluoro-2-pyridin-3-yl-1H-indole (Example 86, 276 mg, 1.12 mmol) in DMF (4 mL) is added 60% sodium hydride in mineral oil (120 mg, 3.0 mmol) and the suspension is stirred for 30 min. Iodomethane (213 mg, 1.5 mmol) is then added to the reaction mixture and stirred at ambient temperature for 1 h. Water (2 mL) is added to quench the reaction. The mixture is filtered and purified by HPLC using Xbridge C18 with a gradient of acetonitrile in 0.1% NH4OH to afford 5-chloro-7-fluoro-1-methyl-2-pyridin-3-yl-1H-indole. MS (ESI) m/z 261 (M+H)+.

후처리

  1. stirringstirred at ambient temperature for 1 h
  2. customto quench
  3. customthe reaction
  4. filtrationThe mixture is filtered
  5. custompurified by HPLC

출처 및 근거

ORD 기록
ord-42aa36411c00462e9194c3a276044504
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030334B2

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