Methyl iodide → HCID 21706269、化合物

HRID 1594921ノート

反応式

HRID 1594921 の反応式
[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

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 12665502HCID 12665502、化合物

生成物 1

HCID 21706269HCID 21706269、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-aaf4ccc0e3c8452784d6d35bff1438ff
出典データセット
uspto-grants-2001_09
特許番号
US06284755B1

反応ノート

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