HRID30107

反应详情

EQUATION

反应方程式

HRID 30107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-[6-Amino-5-(2-fluoro-benzoyl)-pyridin-2-ylamino]-piperidine-1-carboxylic acid tert-butyl ester (269.6 mg, 0.6504 mmol, Example 8) was dissolved in dichloromethane (5 mL), cooled to 0° C. and treated with trifluoroacetic acid (2.5 mL). After stirring ˜30 minutes, the reaction mixture was concentrated in vacuo. The salt was then neutralized with saturated sodium carbonate (˜3 mL), extracted with ethyl acetate/methylene chloride (˜50 mL), washed with saturated sodium chloride (˜3 mL), dried over sodium sulfate and evaporated in vacuo to give [2-Amino-6-(piperidin-4-ylamino)-pyridin-3-yl]-(2-fluoro-phenyl)-methanone as an off-white solid (200 mg, 0.636 mmol, 98 % yield).

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. extractionextracted with ethyl acetate/methylene chloride (˜50 mL)
  3. washwashed with saturated sodium chloride (˜3 mL)
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo