HRID1919899
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
Methyl 4-{3-tert-butoxy-2-[(tert-butoxycarbonyl)amino]-3-oxopropyl}benzoate (0.40 g, 1.05 mmol) was dissolved in THF (10 mL). KOSiMe3 (0.27 g, 2.10 mmol) was added to the solution and allowed to stir overnight at room temperature under nitrogen. Saturated ammonium chloride was added and allowed to stir. Hydrochloric acid (2 mL, 1M solution) was added. The reaction was diluted with ethyl acetate and separated. The aqueous layer was extracted three times with ethyl acetate. The combined organic layer was dried with sodium sulfate, filtered, and concentrated. The resulting material was purified by HPLC. MS: cal'd 365 (MH+), exp 388 (MH+).
WORKUP
后处理
- stirringto stir
- customseparated
- extractionThe aqueous layer was extracted three times with ethyl acetate
- dry with materialThe combined organic layer was dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe resulting material was purified by HPLC