Hydrochloric Acid → 4-Propylpyridin-2-amine

HRID 1038545

反応式

HRID 1038545 の反応式
[CH2:1]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][CH:5]=1)[CH2:2][CH3:3].[NH2-:10].[Na+].Cl>C1(C)C=CC=CC=1>[CH2:1]([C:4]1[CH:9]=[CH:8][N:7]=[C:6]([NH2:10])[CH:5]=1)[CH2:2][CH3:3]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24533Sodium amideHCID 707384-Propylpyridine

生成物 1

HCID 70225944-Propylpyridin-2-amine収率 51%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
140 °C

実験手順

To a solution of 4-propylpyridine (10.0 g, 82.5 mmol) in toluene (170 mL), sodium amide (6.4 g, 165 mmol) was added at room temperature, and the mixture was stirred at 140° C. for 2 days. Under ice-cold conditions, the reaction solution was added 6N aqueous solution of hydrochloric acid (30 mL), and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate/1% triethylamine), and the title compound (5.70 g (yield 51%)) was obtained as a red-brown solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe obtained residue was purified by silica-gel column chromatography (hexane/ethyl acetate/1% triethylamine)

出典と根拠

ORDレコード
ord-a03d1944fe274bf393149e71d3fdb1fd
出典データセット
uspto-grants-2013_10
特許番号
US08551985B2

関連ノート

読み込み中…