HRID78140

反应详情

EQUATION

反应方程式

HRID 78140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of lithium aluminum hydride (689 mg, 14.5 mmol, purity: 80%) in tetrahydrofuran (20 mL) was added 5-phenoxy-nicotinic acid methyl ester (1.11 g, 4.84 mmol) described in Manufacturing Example 145-1-1 at 0° C., which was stirred for 20 minutes at room temperature. First water (689 mL), then a 5 N sodium hydroxide aqueous solution (689 μL), and then water (2.07 mL) were added at 0° C. to the reaction mixture, which was filtered through a Celite pad. The filtrate was concentrated under a reduced pressure, and the residue was purified by NH silica gel column chromatography (heptane: ethyl acetate=1:1) to obtain the title compound (756 mg, 78%).

WORKUP

后处理

  1. customdescribed in Manufacturing Example 145-1-1 at 0° C.
  2. filtrationwas filtered through a Celite pad
  3. concentrationThe filtrate was concentrated under a reduced pressure
  4. customthe residue was purified by NH silica gel column chromatography (heptane: ethyl acetate=1:1)