HRID2269309
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 refluxing mixture of rhodium acetate dimer (0.0093 g, 0.02 mmol) and 40 mL of benzene was added dropwise a solution of 2-tert-butoxycarbonylamino-5-diazo-4-oxo-pentanoic acid methyl ester (0.60 g, 2.1 mmol) in 4.5 mL of benzene. After stirring for 2 h at reflux, the mixture was cooled to room temperature, concentrated in vacuo, and filtered through a small pad of silica gel eluting with 1:1 ethyl acetate-hexane. Concentration of the filtrate afforded 0.53 g of 4-oxo-piperidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester as a yellow oil.
WORKUP
后处理
- temperatureat reflux
- concentrationconcentrated in vacuo
- filtrationfiltered through a small pad of silica gel eluting with 1:1 ethyl acetate-hexane