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

HRID 1360708노트

반응식

HRID 1360708 반응식
[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

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 16065181HCID 16065181, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e69dd940723e4bf2b684f1f2c44d273d
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07879875B2

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