تفاعل #40942

ord-6cb627a6ee604040bc5f5bdbf9aeff00

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلthe solution was washed with aqueous saturated NaHCO3 solution
  2. 2
    تجفيفThe organic phase was dried (Na2SO4)
  3. 3
    أخرىevaporated
  4. 4
    أخرىThe crude was purified by flash chromatography with ethyl acetate-petroleum ether (7-3)

الإجراء التجريبي

1-(3-Hydroxy-propyl)-5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione (Prep 28.36 mg, 0.13 mmol) was dissolved in dry THF (5 mL), the solution was cooled to 0° C. and then Dess-Martin periodinane (97 mg, 0.22 mmol) was added under nitrogen. The mixture was stirred at room temperature for 1.5 hours. Ethyl acetate was added and the solution was washed with aqueous saturated NaHCO3 solution. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with ethyl acetate-petroleum ether (7-3) to give 17 mg of the title compound (50% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07727988B2uspto-grants-2010_06