HRID1291236

反应详情

EQUATION

反应方程式

HRID 1291236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

Under argon gas, 7H-pyrrolo[2,3-d]pyrimidin-4(3H)-one (1.0 g) was dissolved in DMF (35 ml) with warming. Then, anhydrous potassium carbonate (1.02 g) and isopropyl iodide (1.1 ml) were added and the mixture was stirred at 55° C. for 13 hours. The insoluble matter was filtered off and the solvent was distilled off under reduced pressure. The residue was purified by flash column chromatography (silica gel; hexane: ethyl acetate=4:1→1:1) to provide the title compound (110 mg). 1 H-NMR (CDCl3) δ: 1.48(6H,d,J=7.OHz), 5.31(1H,m), 6.74(1H,dd,J=2.2&3.4Hz), 6.96(1H,dd,J=2.2&3.4Hz), 7.95(1H,s), 9.20(1H,brs).

WORKUP

后处理

  1. temperaturewith warming
  2. filtrationThe insoluble matter was filtered off
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by flash column chromatography (silica gel; hexane: ethyl acetate=4:1→1:1)