HRID33977

反应详情

EQUATION

反应方程式

HRID 33977 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 2-(N′-methoxy-N′-methylaminocarbonylmethylamino)-3-methyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one (1.46 g, 3.4 mmol) in THF (30 mL) at 0° C. was slowly added benzylmagnesium chloride (Aldrich, 2.5M in THF, 20 mL). After 2 h, water (100 mL) and ethyl acetate (200 mL) were added. The layers were separated. The organic layer was washed with brine (3×80 mL), dried, and evaporated to give the crude product. Column chromatograph purification (silica gel, 1-2% MeOH/CH2Cl2) gave the final product. M+1=491.2.

WORKUP

后处理

  1. customat 0° C.
  2. customThe layers were separated
  3. washThe organic layer was washed with brine (3×80 mL)
  4. customdried
  5. customevaporated
  6. customto give the crude product
  7. customColumn chromatograph purification (silica gel, 1-2% MeOH/CH2Cl2)