HRID1368526

反应详情

EQUATION

反应方程式

HRID 1368526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

4-[1-Methoxy-1-(6-methoxynaphthalen-2-yl)ethyl]-1-trityl-1H-imidazole (1.5 g) and pyridine hydrochloride (500 mg) were dissolved in methanol (8 ml). The solution was stirred at 60° C. for 2 h. After cooling, 1 N-hydrochloric acid was added to the solution, and precipitate was filtered off. The filtrate was washed with ether and neutralized with potassium carbonate. The filtrate was extracted with ethyl acetate, washed with saturated aqueous solution of sodium chloride, dried and concentrated. The residue was purified by silica gel column chromatography (eluent, ethyl acetate:methanol=30:1) to give the titled compound (0.33 g) as a colorless powder.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationwas filtered off
  3. washThe filtrate was washed with ether and neutralized with potassium carbonate
  4. extractionThe filtrate was extracted with ethyl acetate
  5. washwashed with saturated aqueous solution of sodium chloride
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was purified by silica gel column chromatography (eluent, ethyl acetate:methanol=30:1)