HRID1404316
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
In another reaction vessel, 96.2 g (394 mmol) of 4-trimethylsilyloxy-2,2,6,6-tetramethylpiperidine-N-oxide was dissolved in 100 ml of dehydrated THF, and the Grignard reactant prepared was dropped at 0° C. After a reaction for 3 hours, the solution was concentrated by a rotary evaporator. 500 mL of water was added to the residue and an extraction was carried out using 500 mL in total of ethyl acetate, and the organic layer was concentrated by a rotary evaporator. The residue was purified by column chromatography (silica gel, hexane/ethyl acetate=20/1, volume ratio) to obtain 38.5 g of 1-(1-propyl)oxy-2,2,6,6-tetramethyl-4-trimethylsilyloxypiperidine.
WORKUP
后处理
- additionwas dropped at 0° C
- customAfter a reaction for 3 hours
- concentrationthe solution was concentrated by a rotary evaporator
- addition500 mL of water was added to the residue
- extractionan extraction
- concentrationthe organic layer was concentrated by a rotary evaporator
- customThe residue was purified by column chromatography (silica gel, hexane/ethyl acetate=20/1, volume ratio)