HRID18713
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-(2-fluorophenyl)imidazolidine-2-thione (26) (2.45 g, 0.0084 mol) and methyl iodide (0.79 mL, 0.012 mol) in abs. EtOH (30 mL) is heated at 90° C. overnight. The reaction mixture is cooled to rt, concentrated in vacuo, and the residue crystallized from abs EtOH/Et2O to give 3.42 g of the product 43. 1H NMR (DMSO-d6) δ 10.85 (s, 2 H), 7.30-7.10 (m, 4 H), 7.10-6.90 (m, 4 H), 6.04 (s, 2 H), 2.80 (s, 3 H); MS: m/z 305 (M++1).
WORKUP
后处理
- concentrationconcentrated in vacuo
- customthe residue crystallized from abs EtOH/Et2O