Methyl iodide → 6-(2,4-difluorophenyl)-1-(2,6-difluorophenyl)-7-(methoxymethyl)-2H-quinolizin-2-one

HRID 1360708ノート

反応式

HRID 1360708 の反応式
[H-].[Na+].I[CH3:4].[F:5][C:6]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:7]=1[C:13]1[N:14]2[C:19]([CH:20]=[CH:21][C:22]=1[CH2:23][OH:24])=[C:18]([C:25]1[C:30]([F:31])=[CH:29][CH:28]=[CH:27][C:26]=1[F:32])[C:17](=[O:33])[CH:16]=[CH:15]2>C1COCC1>[F:5][C:6]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:7]=1[C:13]1[N:14]2[C:19]([CH:20]=[CH:21][C:22]=1[CH2:23][O:24][CH3:4])=[C:18]([C:25]1[C:26]([F:32])=[CH:27][CH:28]=[CH:29][C:30]=1[F:31])[C:17](=[O:33])[CH:16]=[CH:15]2

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 16065181HCID 16065181、化合物

生成物 1

HCID 160653126-(2,4-difluorophenyl)-1-(2,6-difluorophenyl)-7-(methoxymethyl)-2H-quinolizin-2-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Oil free sodium hydride suspended in THF was added iodomethane (0.06 mL) and 6-(2,4-difluorophenyl)-1-(2,6-difluorophenyl)-7-(hydroxymethyl)-2H-quinolizin-2-one (Example 50, 40 mg) at 0° C. The mixture was warmed to room temperature and stirred for a couple of hours until reaction complete. The mixture was quenched with water, extracted with ethyl acetate, brine, dried over MgSO4 and concentrated. The residue was purified by silica gel (100% acetone) to give the title compound (22 mg).

後処理

  1. customThe mixture was quenched with water
  2. extractionextracted with ethyl acetate, brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel (100% acetone)

出典と根拠

ORDレコード
ord-e69dd940723e4bf2b684f1f2c44d273d
出典データセット
uspto-grants-2011_02
特許番号
US07879875B2

反応ノート

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