反应 #1144434

ord-8cc9ce0ee045418088ce1a2501c1672c

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heated
  2. 2
    温度under reflux for 15 hours
  3. 3
    过滤filtered through Celite
  4. 4
    洗涤The organic layer was washed with water
  5. 5
    其他dried on magnesium sulfate
  6. 6
    浓缩concentrated under reduced pressure
  7. 7
    其他The residue was crystallized from ethyl acetate

实验过程

To 100 ml of methylene chloride, 5.1 g (40 mmol) of 5-ethyluracil and 22 ml (88 mmol) of bistrimethylsilylacetamide were added under a nitrogen atmosphere and stirred for 40 minutes at room temperature. To this mixture, 4.1 ml (88 mmole) of chloromethyl ethyl ether and 0.15 g (0.4 mmol) of tetrabutylammonium iodide were added and heated under reflux for 15 hours. Then, the reaction mixture was poured into 50 ml of saturated sodium bicarbonate solution carefully and filtered through Celite. The organic layer was washed with water, dried on magnesium sulfate and concentrated under reduced pressure. The residue was crystallized from ethyl acetate to obtain 6.4 g of 1-ethoxymethyl-5-ethyluracil (Yield: 81%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE037979E1uspto-grants-2003_02