反応 #168587

反応方程式

isobutyl iodide

6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione

isobutyl iodide

potassium carbonate

→

pure product

収率 52.0%

6-Chloro-1-isobutyl-3-methylpyrimidine-2,4(1H,3H)-dione

収率 52.0%

溶媒

DMF

反応条件

後処理

1. 1
   温度the reaction mixture heated at 50° C. for 24 hours
2. 2
   ろ過After hot filtration
3. 3
   その他the filtrate is evaporated to dryness under reduced pressure
4. 4
   その他The obtained oil is further purified by silica-gel flash chromatography

実験手順

A mixture of 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione (3 g, 18.8 mmol), isobutyl iodide (5 mL, 43.5 mmol) and potassium carbonate (5.3 g, 38.4 mmol) in anhydrous DMF (200 mL) is heated at 50° C. for 8 hours. Additional isobutyl iodide (4.3 mL, 37.5 mmol) is added, and the reaction mixture heated at 50° C. for 24 hours. After hot filtration, the filtrate is evaporated to dryness under reduced pressure. The obtained oil is further purified by silica-gel flash chromatography to give 2.1 g of pure product (Yield: 52%).

出典