HRID132925
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
A solution of 342 mg (1 mmol) of 4-(2-chloro-6-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester in 5.0 mL of MeOH was treated with 630 mg (10 mmol, 10 eq) of ammonium formate and a catalytic amount of 10% Pd—C (34 mg). The reaction mixture was stirred at 65° C. for 30 min. The reaction mixture was then filtered through a pad of celite and concentrated to obtain a yellow solid. TLC (silica, 5% acetone/CH2Cl2): Rf=0.40. MS (electrospray): exact mass calculated for C15H22ClN3O2, 311.14; m/z found, 312.1 [M+H]+.
WORKUP
后处理
- filtrationThe reaction mixture was then filtered through a pad of celite
- concentrationconcentrated
- customto obtain a yellow solid