Pentylamine → N-[(2'-nitro-1,1'-biphenyl-4-yl)methyl]-N-pentylamine

HRID 492289

反応式

HRID 492289 の反応式
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][NH2:6].C(=O)([O-])[O-].[K+].[K+].[N+:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22]1[CH:27]=[CH:26][C:25]([CH2:28]Br)=[CH:24][CH:23]=1)([O-:15])=[O:14].C(OCC)(=O)C>CN(C)C=O>[N+:13]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22]1[CH:27]=[CH:26][C:25]([CH2:28][NH:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])=[CH:24][CH:23]=1)([O-:15])=[O:14]

参加物

6

反応物 4

HCID 8060PentylamineHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 117790721,1'-Biphenyl, 4'-(bromomethyl)-2-nitro-

生成物 1

HCID 17860716N-[(2'-nitro-1,1'-biphenyl-4-yl)methyl]-N-pentylamine収率 77%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

n-Amylamine (0.54 g) and potassium carbonate (0.98 g) were suspended in dimethylformamide (3.5 mL), and [[2′-nitro-1,1′-biphenyl-4-yl]methyl] bromide (0.51 g) was added in portions. Four hours later, ethyl acetate (20 mL) was added, and the resulting mixture was washed once with water (40 mL) and twice with brine (90 mL, each). The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was subjected to chromatography on a silica gel column (chloroform/ethyl acetate) to afford N-[(2′-nitro-1,1′-biphenyl-4-yl)methyl]-N-pentylamine as a yellow oil (0.40 g). Yield: 77%.

後処理

  1. washthe resulting mixture was washed once with water (40 mL) and twice with brine (90 mL
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2f06d0472f194e309a6ff5cff80b3326
出典データセット
uspto-grants-2009_05
特許番号
US07531576B2

関連ノート

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