Methyl iodide → HCID 21706269, 화합물

HRID 1594921노트

반응식

HRID 1594921 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]2[NH:15][C:14](=[O:16])[CH2:13][CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.[H-].[Na+].I[CH3:20]>C1COCC1>[CH3:20][C:5]1([CH:9]2[NH:15][C:14](=[O:16])[CH2:13][CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH2:4]1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 12665502HCID 12665502, 화합물

생성물 1

HCID 21706269HCID 21706269, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

7-(3-Methoxyphenyl)-azepan-2-one, as described above in Step C, (0.13 g, 0.6 mmol) and NaH (60% dispersion in mineral oil) (0.03 g, 0.75 mmol) were dissolved in THF (5 mL) under Ar at ambient temperature. After 0.25 hours, iodomethane (0.064 mL, 1.0 mmol) was added and stirring was continued for 20 h. The reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL), the organic layer separated, washed with H2O, dried (MgSO4), filtered and concentrated to give the title compound after SiO2 chromatography (CHCl3:MeOH, 100:1 to 50:1).

후처리

  1. waitwas continued for 20 h
  2. customThe reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL)
  3. customthe organic layer separated
  4. washwashed with H2O
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-aaf4ccc0e3c8452784d6d35bff1438ff
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06284755B1

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