HRID535779

反应详情

EQUATION

反应方程式

HRID 535779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(2-Amino-3,3-dimethylbutanoyl)benzonitrile hydrochloride (Example 3, 50 mg, 0.23 mmol) was added to a solution of CDI (112 mg, 0.69 mmol) and TEA (0.035 mL, 0.25 mmol) in MeCN (5 mL). The reaction mixture was stirred at rt for 90 minutes before 1-(6-methylpyridin-2-yl)piperazine (CAS 55745-89-6, 205 mg, 1.16 mmol) was added. The mixture was stirred for 1 h and the solvent was evaporated under reduced pressure. The product was dissolved in methanol, filtered and purified by prep. HPLC yielding N-(1-(4-cyanophenyl)-3,3-dimethyl-1-oxobutan-2-yl)-4-(6-methylpyridin-2-yl)piperazine-1-carboxamide (36.3 mg, 37%).

WORKUP

后处理

  1. additionwas added
  2. customthe solvent was evaporated under reduced pressure
  3. dissolutionThe product was dissolved in methanol
  4. filtrationfiltered
  5. custompurified by prep