4-Fluorobenzonitrile → N-(4-Cyanophenyl)-4-piperidone propylene ketal

HRID 842784ノート

反応式

HRID 842784 の反応式
F[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[CH2:10]1[O:20][C:14]2([CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[O:13][CH:11]1[CH3:12]>ClCCl.C(=O)([O-])[O-].[Na+].[Na+]>[CH2:10]1[O:20][C:14]2([CH2:19][CH2:18][N:17]([C:2]3[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=3)[CH2:16][CH2:15]2)[O:13][CH:11]1[CH3:12]

参加物

5

反応物 2

HCID 145174-FluorobenzonitrileHCID 129541174-Piperidone propylene ketal

生成物 1

HCID 57228643N-(4-Cyanophenyl)-4-piperidone propylene ketal

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 10340Sodium Carbonate溶媒

実験手順

A mixture of 4-fluorobenzonitrile (1.22 g, 10.0 mmol) and 4-piperidone propylene ketal (2.02 g, 12.85 mmol) was stirred at room temperature overnight. The resulting mixture was diluted with dichloromethane and sodium carbonate solution and the aqueous layer was extracted with two additional portions of dichloromethane. The combined organic extracts were washed with brine and dried over Na2SO4. The solvent was removed in vacuo. PCTLC (SiO2, 6 mm, 10% EtOH-90% CHCl3) afforded the title compound (34).

後処理

  1. extractionthe aqueous layer was extracted with two additional portions of dichloromethane
  2. washThe combined organic extracts were washed with brine
  3. dry with materialdried over Na2SO4
  4. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-e3f82736699c42a688c96bdd22b6876d
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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