反应 #1824320

ord-4ca98fb0e6f6433e8d78c63ea080cf22

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONare added
  2. 2
    洗涤washed three times with 2% aqueous citric acid, saturated sodium hydrogencarbonate solution
  3. 3
    干燥After drying above sodium sulfate
  4. 4
    其他the solvent is evaporated under reduced pressure
  5. 5
    其他The oily residue is crystallized by trituration with diethyl ether

实验过程

13.42 g (0.1 mol) of 2,5-dithia cyclohexanone dissolved in 250 ml of anhydrous dichloromethane are added by dropping, and in an argon atmosphere, to a solution of 29.79 g (0.1 mol) of cysteine decyl ester hydrochloride and 10.12 g (0.1 mol) of triethyl amine in 500 ml of anhydrous dichloromethane. The reaction mixture is kept agitated overnight at room temperature and then washed three times with 2% aqueous citric acid, saturated sodium hydrogencarbonate solution and with water. After drying above sodium sulfate, the solvent is evaporated under reduced pressure. The oily residue is crystallized by trituration with diethyl ether.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05961954uspto-grants-1999_10