HRID1795793
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
- 100 °C
PROCEDURE
实验过程
A stirred mixture of oxalyl chloride (5.3 mL, 60 mmol) and benzyl-N-(1-cyanoethyl)glycine hydrochloride (3.82 g, 15 mmol), as prepared in the preceding step, in 1,2-dichlorobenzene (30 mL) was heated to 100° C. overnight. The solvent was evaporated in vacuo and the residue was purified by flash column chromatography to give a solid. 10% Ethyl acetate in hexane (100 mL) was added and the solid was collected to give the title compound as an orange crystalline solid (2.7 g, 55%). 1H NMR (CDCl3) δ 7.38 (m, 5 H), 5.24 (s, 2 H), 4.89 (s, 2 H), 2.34 (s, 3 H).
WORKUP
后处理
- customThe solvent was evaporated in vacuo
- customthe residue was purified by flash column chromatography
- customto give a solid
- customthe solid was collected