Isopropyl iodide → 1-Isopropyl-4-(4-nitrophenyl)piperidine

HRID 605965

反応式

HRID 605965 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].C([O-])([O-])=O.[K+].[K+].I[CH:23]([CH3:25])[CH3:24]>C(#N)C>[CH:23]([N:13]1[CH2:12][CH2:11][CH:10]([C:7]2[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[CH2:15][CH2:14]1)([CH3:25])[CH3:24]

参加物

5

反応物 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 159258174-(4-Nitrophenyl)piperidine

生成物 1

HCID 574241751-Isopropyl-4-(4-nitrophenyl)piperidine収率 99.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4-(4-Nitrophenyl)piperidine (250 mg, 1.21 mmol), K2CO3 (170 mg, 1.21 mmol) and 2-iodopropane (240 μL, 2.4 mmol) are stirred in acetonitrile (3 mL) in a sealed tube at 120° C. for 45 min. The mixture is cooled and the solvent removed under reduced pressure. The residue is partitioned between DCM (20 mL) and water (5 mL), the layers are separated and the DCM is washed with water (5 mL) and brine (5 mL) and dried over MgSO4. Evaporation of the solvent affords the title compound (300 mg) which is used without further purification.

後処理

  1. temperatureThe mixture is cooled
  2. customthe solvent removed under reduced pressure
  3. customThe residue is partitioned between DCM (20 mL) and water (5 mL)
  4. customthe layers are separated
  5. washthe DCM is washed with water (5 mL) and brine (5 mL)
  6. dry with materialdried over MgSO4
  7. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-41702c0ab2ef4bde83af5a601535e51b
出典データセット
uspto-grants-2011_03
特許番号
US07915256B2

関連ノート

読み込み中…