HCID 22398528、化合物 → 4-(5-Fluoro-2-methoxyphenyl)-4-methylpentan-2-one

HRID 916022ノート

反応式

HRID 916022 の反応式
[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

参加物

4

反応物 2

HCID 22398528HCID 22398528、化合物HCID 178418348HCID 178418348、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d156692828644d96932c461e2b2ae425
出典データセット
uspto-grants-2007_09
特許番号
US07268152B2

反応ノート

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