HRID10077
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
3-Ethylamino-4-methyl-phenol (0.3 g, 2 mmol) and benzo[de]isochromene-1,3-dione (0.2 g, 1 mmol) in sulfuric acid (3 ml) was heated to 150° C. over a period of 6 h. The reaction mixture was pouring into crushed ice, allowed to stand over a period of 1 h and the precipitate was filtered. The filtrate was neutralized with concentrated ammonium hydroxide and concentrated to give a dark purple residue. Purification via preparatory layer chromatography (PLC, 1 mm silica gel, 9/1 DCM: MeOH, 2% AcOH) gave the title compound (50 mg). ABS λmax=527 nm (EtOH).
WORKUP
后处理
- additionThe reaction mixture was pouring
- custominto crushed ice
- filtrationthe precipitate was filtered
- concentrationconcentrated
- customto give a dark purple residue
- customPurification via preparatory layer chromatography (PLC, 1 mm silica gel, 9/1 DCM: MeOH, 2% AcOH)