反応 #67577

反応方程式

2-Bromopyridine

methylhydrazine

methylhydrazine

→

N-Methyl-N-pyridin-2-yl-hydrazine

収率 74.4%

反応条件

後処理

1. 1
   その他fitted with a water-condenser
2. 2
   その他After a few minutes a vigorous exothermic reaction
3. 3
   その他the excess methylhydrazine was removed under reduced pressure
4. 4
   抽出the resulting solution was extracted with ether (3×100 ml)
5. 5
   乾燥The combined extracts were dried (K2CO3)
6. 6
   その他purified by silica gel chromatography 0-3% EtOH/CH2Cl2

実験手順

2-Bromopyridine (5 mL, 52.4 mmol) and methylhydrazine (20 mL, 360 mmol) were mixed together in a flask fitted with a water-condenser. After a few minutes a vigorous exothermic reaction occurred with refluxing of the methylhydrazine. When the reaction had subsided, the mixture was left for 16 hours, and the excess methylhydrazine was removed under reduced pressure. The cooled residue was stirred with aqueous sodium hydroxide solution (30 ml of 20%), and the resulting solution was extracted with ether (3×100 ml). The combined extracts were dried (K2CO3) and purified by silica gel chromatography 0-3% EtOH/CH2Cl2 to give 4.8 g of N-Methyl-N-pyridin-2-yl-hydrazine.

出典