HRID1493041

反应详情

EQUATION

反应方程式

HRID 1493041 的结构方程式

PROCEDURE

实验过程

4-Amino-2,3,5-trimethylphenol (2.0 g, 13.2 mmol) and 2-methyl-2-propenol (1.15 g, 15.8 g) were heated under reflux in dichloromethane (20 ml) together with sulfuric acid (2 ml) for 18 hours. The reaction mixture was washed with aqueous saturated sodium bicarbonate solution, dried and then concentrated. The residue was purified by silica gel column chromatography (isopropyl ether). The purified product was converted into its hydrochloride and it was crystallized from ethanol-isopropyl ether to obtain the desired compound (460 mg, yield: 14.4%), m.p. 248°-250° C.

WORKUP

后处理

  1. washThe reaction mixture was washed with aqueous saturated sodium bicarbonate solution
  2. customdried
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel column chromatography (isopropyl ether)
  5. customwas crystallized from ethanol-isopropyl ether