HCID 22398528, 화합물 → 4-(5-Fluoro-2-methoxyphenyl)-4-methylpentan-2-one

HRID 916022노트

반응식

HRID 916022 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:20][CH3:21])=[C:6]([C:8]([CH3:19])([CH3:18])[CH2:9][C:10](N2CCOCC2)=[O:11])[CH:7]=1.[CH3:22][Li]>C1COCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:20][CH3:21])=[C:6]([C:8]([CH3:18])([CH3:19])[CH2:9][C:10](=[O:11])[CH3:22])[CH:7]=1

참가 물질

4

반응물 2

HCID 22398528HCID 22398528, 화합물HCID 178418348HCID 178418348, 화합물

생성물 1

HCID 222849224-(5-Fluoro-2-methoxyphenyl)-4-methylpentan-2-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of the above 3-(5-fluoro-2-methoxyphenyl)-3-methyl-1-morpholin-4-ylbutan-1-one (0.59 g) in THF (1 mL) stirred under argon and cooled on dry ice/acetone was added methyl lithium (1.4 M in pentane, 2 mL) over 2 minutes. The mixture was stirred for 30 minutes and quenched with EtOH (0.3 mL). The mixture was warmed to room temperature and 1 mL of water was added. The organic phase was separated, washed, dried, filtered, and evaporated. The residue was fractionated over a short column of silica gel (eluent:hexanes-methylene chloride (1:1)) to give 4-(5-fluoro-2-methoxyphenyl)-4-methylpentan-2-one as an oil (0.36 g).

후처리

  1. temperaturecooled on dry ice/acetone
  2. customquenched with EtOH (0.3 mL)
  3. addition1 mL of water was added
  4. customThe organic phase was separated
  5. washwashed
  6. customdried
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-d156692828644d96932c461e2b2ae425
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268152B2

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