HRID1772679
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
To a solution of ethyl 3-hydroxycyclobutanecarboxylate (10.2 g, 78.4 mmol) in dry pyridine (56.5 mL) at 0° C., TsCl (14.9 g, 78.4 mmol) was added portionwise. The resulting mixture was stirred at rt overnight. The reaction mixture was concentrated under reduced pressure and the residue obtained was dissolved in EtOAc (100 mL) and sequentially washed with 2 N HCl (100 mL), saturated NaHCO3 (100 mL) and water (100 mL). The EtOAc layer was dried over Na2SO4, filtered, and concentrated to obtain ethyl 3-(tosyloxy)cyclobutanecarboxylate as a pale yellow oil, which was used in the next step without further purification.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- customthe residue obtained
- washsequentially washed with 2 N HCl (100 mL), saturated NaHCO3 (100 mL) and water (100 mL)
- dry with materialThe EtOAc layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated