Sodium Iodide → N-(4-nitrobenzyl)-N-(2-pyrimidinyl)amine

HRID 24925

反応式

HRID 24925 の反応式
Cl.[N+:2]([C:5]1[CH:12]=[CH:11][C:8]([CH2:9][NH2:10])=[CH:7][CH:6]=1)([O-:4])=[O:3].C(=O)([O-])[O-].[Na+].[Na+].[I-].[Na+].Cl[C:22]1[N:27]=[CH:26][CH:25]=[CH:24][N:23]=1>C(O)C>[N:23]1[CH:24]=[CH:25][CH:26]=[N:27][C:22]=1[NH:10][CH2:9][C:8]1[CH:7]=[CH:6][C:5]([N+:2]([O-:4])=[O:3])=[CH:12][CH:11]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 744042-ChloropyrimidineHCID 112524674-Nitrobenzylamine hydrochloride

生成物 1

HCID 22569285N-(4-nitrobenzyl)-N-(2-pyrimidinyl)amine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

9.4 g (50 mmol) of 4-nitrobenzylamine-hydrochloride, 11.7 g (110 mmol) of sodium carbonate and 7.5 g (50 mmol) of sodium iodide are added to a solution of 5.7 g (50 mmol) of 2-chloropyrimidine in 250 ml of ethanol. The mixture is refluxed for 20 hours. Then the salts are removed by suction filtering, the filtrate is evaporated down and taken up in 300 ml of ethyl acetate. It is washed with water, the solvent is eliminated in vacuo and the residue is chromatographed on silica gel (dichloromethane/methanol=97:3).

後処理

  1. temperatureThe mixture is refluxed for 20 hours
  2. customThen the salts are removed by suction
  3. filtrationfiltering
  4. customthe filtrate is evaporated down
  5. washIt is washed with water
  6. customthe residue is chromatographed on silica gel (dichloromethane/methanol=97:3)

出典と根拠

ORDレコード
ord-ac39fbc2361146da9b0c5a09401c6fad
出典データセット
uspto-grants-2005_02
特許番号
US06855710B2

関連ノート

読み込み中…