HRID583059

反应详情

EQUATION

反应方程式

HRID 583059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Compound 43 (693 mg, 1.98 mmol) was dissolved in concentrated H2SO4 (5 ml) and the mixture was added with KNO3 (240 mg, 2.37 mmol) under ice cooling. After 1 hour, the reaction mixture was poured into ice water and extracted with dichloromethane. The organic phase was washed with saturated aqueous solution of sodium hydrogen carbonate, water and saturated brine, and then concentrated after dryness. The residue was recrystallized from ethyl acetate to give methyl 4-[3-nitro-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-2-naphthylcarbonyl]benzoate as colorless needles (Compound 44, 414 mg, 53%).

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. washThe organic phase was washed with saturated aqueous solution of sodium hydrogen carbonate, water and saturated brine
  3. concentrationconcentrated after dryness
  4. customThe residue was recrystallized from ethyl acetate