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
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
Under a nitrogen gas atmosphere, 0.0096 g (7.3×10-6 mol) of [RuI(p-Cymene)((+)-SO3Na-BINAP)]I, 0.1164 g (7.8×10-4 mol) of NaI, 1 ml (7.5×10-3 mol) of ethyl acetoacetate, and 1.5 ml of water were charged in a 100 milli-liter autoclave. After displacing the inside atmosphere of the autoclave with a hydrogen gas, the autoclave was pressed at a hydrogen pressure of 50 kg/cm2 and the mixture was stirred for 40 hours at 65° C. After the reaction was over, the hydrogen gas was removed, and after added thereto 100 ml of water and 100 ml of ether, the ether extraction was carried out. The ether extract was recovered, dried with anhydrous sodium sulfate, and further ether was distilled off to provide 0.62 g (percent yield 63%) of ethyl 3-hydroxybutyrate. By the analysis of gas chromatography (PEG-HT), the conversion ratio was determined to be 99%.
WORKUP
后处理
- customwas removed
- additionafter added
- extraction100 ml of water and 100 ml of ether, the ether extraction
- extractionThe ether extract
- customwas recovered
- dry with materialdried with anhydrous sodium sulfate, and further ether
- distillationwas distilled off