HRID60493
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of 5-(1-hydroxy-3-methylbutyl)-6-isopropoxy-1-methyl-3-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (60 mg, 0.13 mmol) in HCOOH (2 mL) was added Zn dust (42 mg, 0.65 mmol). The reaction was heated at 80° C. for 1 h, cooled to RT and filtered. The filtrate was concentrated and dried to a residue which was purified by Prep TLC eluted with PE/EA (2:1) to give 3-(5-isopentyl-6-isopropoxy-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate (48 mg, 82.7% yield) as a white solid. LCMS: MH+ 392 and TR=2.964 min.
WORKUP
后处理
- temperaturecooled to RT
- filtrationfiltered
- concentrationThe filtrate was concentrated
- customdried to a residue which
- customwas purified by Prep TLC
- washeluted with PE/EA (2:1)