HRID1632257
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of lithium hexamethyldisilazide was prepared by the addition of 5.12 ml of a 1.6M solution of n-butyllithium in hexane to 1.75 ml of hexamethyldisilazane in 25 ml of dry THF at -10° with stirring, under argon. The solution was cooled to -78° and added by cannula to 1.57 g of 4-nitrobenzyl 2-(4-allylthioazetidin-2-on-1-yl)acetate in 12 ml of dry THF at -78°, with stirring under argon. After 5 minutes 0.846 ml of carbondisulphide was added by syringe. 1.77 ml of acetic anhydride were then added, followed by 1.07 ml of glacial acetic acid. The solution was allowed to warm to room temperature and evaporated to leave an orange oil.
WORKUP
后处理
- temperatureThe solution was cooled to -78°
- stirringwith stirring under argon
- customevaporated
- customto leave an orange oil