HRID18714
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
A mixture of cis-4,5-bis-(3-fluorophenyl)imidazolidine-2-thione (27) (4.5 g, 0.0188 mol) and methyl iodide (1.45 mL, 0.0232 mol) in abs. EtOH (50 mL) is heated at 95° C. overnight. The reaction mixture is cooled to RT, concentrated in vacuo, and the residue suspended in abs EtOH/Et2O. The insoluble material is filtered to give 6.10 g of the product 44. 1H NMR (DMSO-d6) δ 10.78 (s, 2 H), 7.30-7.15 (m, 2 H), 7.05-6.90 (m, 6 H); 5.87 (s, 2 H), 2.87 (s, 3 H); MS: m/z 305 (M++1).
WORKUP
后处理
- concentrationconcentrated in vacuo
- filtrationThe insoluble material is filtered