반응 #88739

반응 방정식

6-bromo-5-((4-chlorophenyl)(hydroxy)methyl)-1-methyl-3-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione

→

3-(6-bromo-5-(4-chlorobenzyl)-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate

수율 73.0%

용매

HCOOH

반응 조건

후처리

1. 1
   온도then cooled to RT
2. 2
   여과filtered
3. 3
   농축The filtrate was concentrated to a residue which
4. 4
   기타was purified by Prep TLC
5. 5
   세척eluted with PE/EA (1:2)

실험 절차

To a solution of 6-bromo-5-((4-chlorophenyl)(hydroxy)methyl)-1-methyl-3-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (300 mg, 0.56 mmol) in HCOOH (10 mL) was added Zn dust (182 mg, 2.78 mmol). The reaction was heated at 60° C. for 1 h then cooled to RT and filtered. The filtrate was concentrated to a residue which was purified by Prep TLC eluted with PE/EA (1:2) to give 3-(6-bromo-5-(4-chlorobenzyl)-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate (190 mg, 73% yield) as a white solid. LCMS: MH+ 468 and TR=1.893 min.

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