反応 #1687634

反応方程式

ammonia

73

N-Acetylmethyl-nicotinamide

P4S10

charcoal

→

5-Methyl-2-(3-pyridyl)-thiazole

溶媒

toluene

反応条件

後処理

1. 1
   温度The suspension was refluxed for 4 h
2. 2
   ろ過filtered
3. 3
   その他The toluene phase was separated
4. 4
   抽出the aqueous phase extracted with 2×100 ml of toluene
5. 5
   乾燥The combined organic phase were dried over MgSO4
6. 6
   その他evaporated in vacuo
7. 7
   その他leaving a heavy, yellow oil, 88

実験手順

To a solution of 8.0 g (0.045 mol) of 73 in 125 ml of toluene, 10 g (0.045 mol) of P4S10 was added. The suspension was refluxed for 4 h and left at room temperature overnight. The mixture was poured into ice water followed by basification with ammonia. The two-phase system was stirred with charcoal and filtered. The toluene phase was separated and the aqueous phase extracted with 2×100 ml of toluene. The combined organic phase were dried over MgSO4 and evaporated in vacuo leaving a heavy, yellow oil, 88. Yield: 2.3 g (0.013 mol), 29%).

出典