HRID567927

反应详情

EQUATION

反应方程式

HRID 567927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 6-(4-nitrophenylmethyl)-3-methyl-1-(2-methylpropyl)thieno[2,3-d]pyrimidin-2,4(1H, 3H)-dione (275 mg) in ethanol (15 ml) and water (1 ml) was added iron powder (82 mg) and ammonium chloride (78 mg). The mixture was heated at 90° C. for 6 h. and then allowed to cool to room temperature. The reaction was filtered and then evaporated before being partitioned between ethyl acetate and water. The organic layer was collected, dried over magnesium sulfate, and then evaporated. The resultant oil was purified by normal phase HPLC (isohexane:ethyl acetate 80-0:20-100) to give the title compound (20 mg).

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. filtrationThe reaction was filtered
  3. customevaporated
  4. custombefore being partitioned between ethyl acetate and water
  5. customThe organic layer was collected
  6. dry with materialdried over magnesium sulfate
  7. customevaporated
  8. customThe resultant oil was purified by normal phase HPLC (isohexane:ethyl acetate 80-0:20-100)