HRID18734

反应详情

EQUATION

反应方程式

HRID 18734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. waitat 45° C. for 3 h
  2. customThe solvent is removed by rotary evaporation
  3. customthe residue crystallized from dichloromethane and Et2O