HRID640116

反应详情

EQUATION

反应方程式

HRID 640116 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 3-trimethylsilanylethynyl-pyridin-2,6-diamine (7.0 g, 34.1 mmol) described in Manufacturing Example 13-1-2 in tetrahydrofuran (100 mL) was added tetrabutylammonium fluoride (1M tetrahydrofuran solution, 17 mL, 17 mmol) on an ice bath, which was stirred for 10 minutes at room temperature. Water was added to the reaction solution, which was then extracted with ethyl acetate 3 times. The extract was dried over sodium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (3.35 g, 73.8%).

WORKUP

后处理

  1. extractionwas then extracted with ethyl acetate 3 times
  2. dry with materialThe extract was dried over sodium sulfate
  3. customthe solvent was evaporated under a reduced pressure
  4. customThe residue was purified by silica gel chromatography (ethyl acetate)