2,4-Dichloropyrimidine → 2-Chloro-4-(2-phenyl-piperidin-1-yl)-pyrimidine

HRID 2252655

反応式

HRID 2252655 の反応式
[C:1]1([CH:7]2[CH2:12][CH2:11][CH2:10][CH2:9][NH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:13][C:14]1[N:19]=[C:18](Cl)[CH:17]=[CH:16][N:15]=1.C(=O)(O)[O-].[Na+]>CCO>[Cl:13][C:14]1[N:19]=[C:18]([N:8]2[CH2:9][CH2:10][CH2:11][CH2:12][CH:7]2[C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:17]=[CH:16][N:15]=1

参加物

5

反応物 3

HCID 775312,4-DichloropyrimidineHCID 1030202-PhenylpiperidineHCID 516892Sodium Bicarbonate

生成物 1

HCID 858366432-Chloro-4-(2-phenyl-piperidin-1-yl)-pyrimidine収率 66%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Phenylpiperidine, Intermediate 15, (0.5 g, 2.52 mmol), 2,4-dichloropyrimidine (0.41 g, 2.77 mmol) and sodium bicarbonate (0.59 g, 5.55 mmol) in dry EtOH (10 mL) were refluxed for 2 hours, under an atmosphere of nitrogen. The mixture was filtered and the filtrate evaporated in vacuo to give a yellow oil. The oil was purified by flash chromatography (EtOAc and isohexane (1:3)/silica) to give the title compound as a colourless oil (46 g, 66%).

後処理

  1. filtrationThe mixture was filtered
  2. customthe filtrate evaporated in vacuo
  3. customto give a yellow oil
  4. customThe oil was purified by flash chromatography (EtOAc and isohexane (1:3)/silica)

出典と根拠

ORDレコード
ord-fe593abc6b7545b989678fed3b8648da
出典データセット
uspto-grants-2008_01
特許番号
US07323464B2

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