Water → 6-(3-Fluoro-benzyloxy)-2-(2-methoxy-1-methyl-ethyl)-3,4-dihydro-2H-isoquinolin-1-one

HRID 2415440노트

반응식

HRID 2415440 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:22]=[CH:23][CH:24]=1)[CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[N:12]([CH:18]([CH3:21])[CH2:19][OH:20])[CH2:11][CH2:10]2.[H-].[Na+].[CH3:27]I.O>CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]([CH:22]=[CH:23][CH:24]=1)[CH2:5][O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[N:12]([CH:18]([CH3:21])[CH2:19][O:20][CH3:27])[CH2:11][CH2:10]2

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 226419476-(3-Fluoro-benzyloxy)-2-(2-hydroxy-1-methyl-ethyl)-3,4-dihydro-2H-isoquinolin-1-one

생성물 1

HCID 226419416-(3-Fluoro-benzyloxy)-2-(2-methoxy-1-methyl-ethyl)-3,4-dihydro-2H-isoquinolin-1-one수율 45.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a mixture of 6-(3-Fluoro-benzyloxy)-2-(2-hydroxy-1-methyl-ethyl)-3,4-dihydro-2H-isoquinolin-1-one (0.020 g, 0.061 mmol) and sodium hydride (55%, 2.2 mg, 0.067 mmol) in N,N′-dimethylformamide (0.2 mL), methyl iodide (0.009 mL, 0.152 mmol) was added. Water was added and the reaction was extracted with ethyl acetate. After drying of the organic layer with MgSO4, filtration and evaporation, the residue was purified by chromatography (SiO2, hexane/ethyl acetate 9:1 v:v) to give the title compound as a white solid (0.0095 g, 43%). MS: m/e=344.4 (M+H+).

후처리

  1. additionwas added
  2. extractionthe reaction was extracted with ethyl acetate
  3. dry with materialAfter drying of the organic layer with MgSO4, filtration and evaporation
  4. customthe residue was purified by chromatography (SiO2, hexane/ethyl acetate 9:1 v:v)

출처 및 근거

ORD 기록
ord-18bbac85ec934774ad02a2ce1af52ec8
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06818774B2

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