HRID60436

反应详情

EQUATION

反应方程式

HRID 60436 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 5-((4-chlorophenyl)(hydroxy)methyl)-1-methyl-6-((6-methylpyridin-3-yl)oxy)-3-(3-((tetrahydro-2H-pyran-2-yl)oxy)propyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (25 mg, 0.046 mmol) in HCOOH (3 mL) was added Zn dust (30.4 mg, 0.46 mmol). The reaction was heated at 70° C. for 40 min, cooled to RT and filtered. The filtrate was concentrated to a residue which was purified by Prep TLC eluted with PE/EA (1:1) to give 3-(5-(4-chlorobenzyl)-1-methyl-6-((6-methylpyridin-3-yl)oxy)-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate (10 mg, 45.8% yield) as a solid. LCMS: MH+ 495 and TR=1.316 min.

WORKUP

后处理

  1. temperaturecooled to RT
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated to a residue which
  4. customwas purified by Prep TLC
  5. washeluted with PE/EA (1:1)