HRID1159186
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
PROCEDURE
实验过程
To 3-(4-chlorophenyl)-propionaldehyde (0.74 g, 4.39 mmol) was added zinc iodide (0.07 g, 0.22 mmol) and trimethylsilyl cyanide (0.522 g, 5.27 mmol) with caution (exothermic reaction). After stirring the mixture at room temperature for 20 min a solution of ammonia in methanol (7N, 4.4 ml, 31 mmol) was added and stirring was continued overnight. The solvent was evaporated and the residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:heptane/ethyl acetate=2:1) to yield a light yellow liquid (0.43 g, 50%); MS (ISP): 195.3 ((M+H)+).
WORKUP
后处理
- customwith caution (exothermic reaction)
- additionwas added
- customThe solvent was evaporated
- customthe residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:heptane/ethyl acetate=2:1)