反应 #1675
ord-4cc12f6af27449db870b9f2027866d61
反应方程式
ammonium chloride
hexane
NaH
pyridinone
1-bromo-2-pentyne
→
product
5-(4-chlorophenyl)-1-(2-pentyn-1-yl)-2-pyrimidinone
溶剂
反应条件
温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.WAITThe resulting mixture was kept at 0° C. for one half hour
- 2萃取The aqueous suspension was extracted with ether (3×100 ml)
- 3洗涤the combined ether layers washed with brine
- 4其他dried
- 5其他yielding the crude product
实验过程
To a suspension of NaH (60% in mineral oil, 340 mg) in dry DMF (75 ml) at 0° C. was added the preceding pyridinone (1.0 g) and the mixture was stirred at 0° C. for one half hour. To the resulting suspension was added 1-bromo-2-pentyne (750 mg) dropwise. The resulting mixture was kept at 0° C. for one half hour and poured into saturated aqueous ammonium chloride (200 ml). The aqueous suspension was extracted with ether (3×100 ml), the combined ether layers washed with brine and dried, yielding the crude product. Trituration with hexane yielded the product as a yellow solid.