HRID2259995

反应详情

EQUATION

反应方程式

HRID 2259995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl (E)-4-[2-(5,6,7,8-tetrahydro-3,5,5,8,8-pentamethylnaphthalen-2-yl)propen-1-yl]-1-N, N-dimethylsulfamoyl-2-imidazolecarboxylate (Compound 4, 0.295 g, 0.605 mmol) was dissolved in a solution of 3M HCl (2.5 mL) and acetone (20 mL) at room temperature and the solution stirred for 30 min. The solution was neutralized with 5% aqueous NaHCO3 and the organic material was extracted with dichloromethane, washed with brine, dried (K2CO3) and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (hexanes/ethyl acetate=3:2) to give the title compound as a light yellow solid (430 mg, 70%).

WORKUP

后处理

  1. extractionthe organic material was extracted with dichloromethane
  2. washwashed with brine
  3. dry with materialdried (K2CO3)
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography on silica gel (hexanes/ethyl acetate=3:2)