反应详情

温度

5 °C

60 g of cystamine hydrochloride are solubilized in 500 mL and cooled to 5° C. pH is raised to 10 by addition of aq. NaOH (30%). A solution of 4-chlorobutanoyl chloride (105 g) in anhydrous THF (500 mL), is added dropwise, while pH is maintained above 7 by addition of aq. NaOH (30%). After completion of the addition and stabilization of pH at 7, the mixture is kept mixing for 3 d. The aqueous layer is extracted with 3×500 mL dichloromethane, combined with THF layer and dried over Na2SO4. After drying under vacuum, 41 g of a white powder are collected. Analyses are in accordance with the expected structure.

1. additionAfter completion of the addition and stabilization of pH at 7
2. additionthe mixture is kept mixing for 3 d
3. extractionThe aqueous layer is extracted with 3×500 mL dichloromethane
4. dry with materialdried over Na2SO4
5. dry with materialAfter drying under vacuum, 41 g of a white powder
6. customare collected