Hydrochloric Acid → 1-(2-Methoxyphenyl)piperidin-4-one

HRID 842777ノート

反応式

HRID 842777 の反応式
C1O[C:4]2([CH2:9][CH2:8][N:7]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[O:16][CH3:17])[CH2:6][CH2:5]2)[O:3]C1.Cl>C(O)(=O)C.O>[CH3:17][O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[N:7]1[CH2:8][CH2:9][C:4](=[O:3])[CH2:5][CH2:6]1

参加物

5

実験手順

A solution of 19 (570 mg, 2.28 mmol) in acetic acid (20 mL), water (20 ml), and concetrated HCl (5 mL) was heated in an oil bath (50° C.) overnight. The solvent was removed in vacuo and the residue dissolved in ether and sodium carbonate solution. The aqueous layer was extracted with two additional portions of ether and the combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. PCTLC (SiO2, 2 mm, CHCl3) afforded the title compound (20)

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in ether
  3. extractionThe aqueous layer was extracted with two additional portions of ether
  4. washthe combined organic extracts were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-78b0210f7a644b369c133b0e1ecf163c
出典データセット
uspto-grants-2002_04
特許番号
US06376503B1

反応ノート

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