Hydrochloric Acid → N-(2-Cyano-4-methylphenyl)-4-piperidone

HRID 842783ノート

反応式

HRID 842783 の反応式
C1O[C:5]2([CH2:10][CH2:9][N:8]([C:11]3[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][C:12]=3[C:18]#[N:19])[CH2:7][CH2:6]2)[O:4]C1C.Cl>CCOCC>[C:18]([C:12]1[CH:13]=[C:14]([CH3:17])[CH:15]=[CH:16][C:11]=1[N:8]1[CH2:9][CH2:10][C:5](=[O:4])[CH2:6][CH2:7]1)#[N:19]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86757963N-(2-Cyano-4-methylphenyl)-4-piperidone propylene ketal

生成物 1

HCID 22615416N-(2-Cyano-4-methylphenyl)-4-piperidone

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A solution of 29 (549 mg, 2.00 mmol) in ether (20 mL) was treated with 3N aqueous HCl (25 mL). The mixture was stirred at room temperature (24 h). The solvent was removed in vacuo and the residue dissolved in 6N HCl (25 mL) and acetic acid (10 mL). The mixture was stirred at room temperature (3 h). The reaction mixture was neutralized with sodium carbonate solution and the aqueous layer was extracted with three portions of ether. The combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure to afford the title compound (30).

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in 6N HCl (25 mL)
  3. stirringThe mixture was stirred at room temperature (3 h)
  4. extractionthe aqueous layer was extracted with three portions of ether
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-87f8721a71604261af6e2c1230d3796f
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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