تفاعل #88702

معادلة التفاعل

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

→

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

المردود 69.7%

المذيبات

HCOOH

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled to RT
2. 2
   ترشيحfiltered
3. 3
   تركيزThe filtrate was concentrated
4. 4
   أخرىdried to a residue which
5. 5
   أخرىwas purified by chromatography
6. 6
   غسيلeluted with PE/EA (10:1 to 1:1)

الإجراء التجريبي

To a solution of 5-((4-chlorophenyl)(hydroxy)methyl)-6-((5-fluoropyridin-3-yl)oxy)-1-methyl-3-(3-((tetrahydro-2H-pyran-2-yl)oxy)propyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (45 mg, 0.092 mmol) in HCOOH (5 mL) was added Zn dust (30.2 mg, 0.462 mmol). The reaction was heated at 70° C. for 1.5 h, cooled to RT and filtered. The filtrate was concentrated and dried to a residue which was purified by chromatography eluted with PE/EA (10:1 to 1:1) to give 3-(5-(4-chlorobenzyl)-6-((5-fluoropyridin-3-yl)oxy)-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate (32 mg, 69.4% yield) as an oil. LCMS: MH+ 499 and TR=1.513 min.

المصدر