HRID640460

反应详情

EQUATION

反应方程式

HRID 640460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a tetrahydrofuran (12 mL) solution of lithium aluminum hydride (706 mg, 14.9 mmol, purity: 80%) was added 2-amino-6-methyl-nicotinic acid ethyl ester (670 mg, 3.72 mmol) described in Manufacturing Example 170-1-2 at 0° C., which was stirred for 30 minutes at room temperature. Water (706 μL), a 5 N sodium hydroxide aqueous solution (706 μL), and water (2.12 mL) were added to the reaction mixture in that order at 0° C., 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 (ethyl acetate:methanol=10:1) to obtain the title compound (379 mg, 74%).

WORKUP

后处理

  1. customdescribed in Manufacturing Example 170-1-2 at 0° C.
  2. filtrationwhich was 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 (ethyl acetate:methanol=10:1)