HRID18734
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
Hydrogen chloride is bubbled into a solution of 85 (0.69 g, 1.58 mmol) in EtOAc (40 mL) for 2 min, and the solution is stirred at RT overnight and then at 45° C. for 3 h. The solvent is removed by rotary evaporation, and the residue crystallized from dichloromethane and Et2O to give 0.52 g of the product 86. 1H NMR (DMSO-d6) δ 9.80-8.40 (m, 3 H), 7.60-7.45 (m, 2 H), 7.35-7.25 (m, 2 H), 7.15-6.95 (m, 6 H), 6.95-6.80 (m, 4 H), 5.50 (s, 2 H), 4.58 (d, 2 H); MS: m/z 346 (M++1).
WORKUP
后处理
- waitat 45° C. for 3 h
- customThe solvent is removed by rotary evaporation
- customthe residue crystallized from dichloromethane and Et2O