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1-Methyl-4-piperidone → 4-[2-(1-Hydroxy-1-methylethyl)phenyl]-1-methylpiperidin-4-ol

HRID 899250
ノート
印刷プレビュー

反応式

HRID 899250 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([OH:11])([CH3:10])[CH3:9].C([Li])CCC.[CH3:17][N:18]1[CH2:23][CH2:22][C:21](=[O:24])[CH2:20][CH2:19]1>O1CCCC1>[OH:11][C:8]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[C:21]1([OH:24])[CH2:22][CH2:23][N:18]([CH3:17])[CH2:19][CH2:20]1)([CH3:10])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 740491-Methyl-4-piperidoneHCID 3295272-(2-Bromophenyl)propan-2-olHCID 178418339Butyllithium

生成物 1

HCID 122896704-[2-(1-Hydroxy-1-methylethyl)phenyl]-1-methylpiperidin-4-ol収率 58%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a stirred solution of 2-(2-bromophenyl)propan-2-ol (step 1, 6.91 g, 32.1 mmol) in tetrahydrofuran (32 mL) was added dropwise a 1.59 M solution of butyllithium in tetrahydrofuran (46.5 mL, 73.9 mmol) at −78° C. for 20 min and the mixture was stirred for 1 h at the same temperature. To the mixture was added dropwise a solution of 1-methylpiperidin-4-one (5.09 g, 45.0 mmol) in tetrahydrofuran (18 mL) at −78° C. for 10 min. This resulting mixture was slowly warmed up to room temperature and stirred for 18 h at the same temperature. The reaction mixture was quenched by the addition of water, and concentrated to give an orange residue. The crude material was partitioned between diethyl ether and water, and then the organic layer washed with brine, dried over sodium sulfate, and evaporated. The residue was purified by column chromatography on silica gel (150 g) eluting with hexane/ethyl acetate (5/1), dichloromethane/methanol (10/1), then dichloromethane/methanol/triethylamine (10/1/1) to afford 4.62 g (58%) of the title compound as a slight yellow syrup:

後処理

  1. stirringstirred for 18 h at the same temperature
  2. customThe reaction mixture was quenched by the addition of water
  3. concentrationconcentrated
  4. customto give an orange residue
  5. customThe crude material was partitioned between diethyl ether and water
  6. washthe organic layer washed with brine
  7. dry with materialdried over sodium sulfate
  8. customevaporated
  9. customThe residue was purified by column chromatography on silica gel (150 g)
  10. washeluting with hexane/ethyl acetate (5/1), dichloromethane/methanol (10/1)

出典と根拠

ORDレコード
ord-1f15b57991e74feea278bd961c581802
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07354925B2

反応ノート

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