HRID1243310
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
Isopropanoyl chloride (112 μL) was added to a mixture of N-tert-butoxycarbonylpiperazine (200 mg) and an excess of potassium carbonate in anhydrous DCM (10 mL) under a nitrogen atmosphere. The mixture was stirred at r.t. for 18 hours, then it was filtered off from inorganics. The organic phase was diluted with Et2O (20 mL) and washed with 1 N hydrochloric acid solution (10 mL). The aqueous phase was made basic with 1N sodium hydroxide solution and extracted twice with DCM. The combined organic layers were dried and concentrated in vacuo and the residue was purified by flash chromatography (AcOEt 100%) to give the title compound (133 mg) as a white solid.
WORKUP
后处理
- filtrationit was filtered off from inorganics
- additionThe organic phase was diluted with Et2O (20 mL)
- washwashed with 1 N hydrochloric acid solution (10 mL)
- extractionextracted twice with DCM
- customThe combined organic layers were dried
- concentrationconcentrated in vacuo
- customthe residue was purified by flash chromatography (AcOEt 100%)