Water → 2-N-methyl-6-fluoro-1-isoquinolinone

HRID 518282

반응식

HRID 518282 반응식
[H-].[Na+].[F:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[NH:9][CH:8]=[CH:7]2.[CH3:15]I.O>CN(C=O)C.C(OCC)(=O)C>[F:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[C:10](=[O:14])[N:9]([CH3:15])[CH:8]=[CH:7]2

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodide2회HCID 24758Sodium hydrideHCID 450908026-Fluoroisoquinolin-1(2H)-one

생성물 1

HCID 693999762-N-methyl-6-fluoro-1-isoquinolinone수율 107.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매2회

실험 절차

Sodium hydride (60% in mineral oil) (211 mg, 5.27 mmol) was added to 6-fluoro-1,2-dihydroisoquinolin-1-one (716 mg, 4.39 mmol) in anhydrous DMF (6 mL) cooled in an ice bath. The mixture was stirred for about 30 min at room temperature and methyl iodide (0.328 mL, 5.27 mmol) was added dropwise. After 1 h, the reaction was judged to be about 60% complete and additional methyl iodide (0.2 mL, 3.2 mmol) was added. After about 1 h, ice and water and ethyl acetate were added to the mixture. After extractive work up with ethyl acetate, the title compound (836 mg) was obtained as a cream solid and carried on without purification.

후처리

  1. temperaturecooled in an ice bath
  2. waitAfter 1 h
  3. waitAfter about 1 h

출처 및 근거

ORD 기록
ord-eb373744b1ed4cd9aa8d85a5a2f98cc3
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115114B2

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