HRID379587

反应详情

EQUATION

反应方程式

HRID 379587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-[(3-hydroxypropyl)thio]-3-methyl-1-(2-methylpropyl)-6-[(pyridin-3-yl)carbonyl]thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (0.35 g, Example 37) in dry ethanol (40 ml) at 0° C. was added sodium borohydride (0.03 g). The reaction was allowed to warm to room temperature and stirred for 2 hours. The solution was concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by normal-phase HPLC eluting with a gradient of 0-5% ethanol in dichloromethane to give the title compound as a white foam. (0.27 g).

WORKUP

后处理

  1. concentrationThe solution was concentrated under reduced pressure
  2. customThe residue was partitioned between ethyl acetate and water
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by normal-phase HPLC
  7. washeluting with a gradient of 0-5% ethanol in dichloromethane