HRID397018
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
300.0 g (1.27 moles) ethyl 4-benzyloxy-3-oxobutyrate, 300 ml ethanol, and 104.5 mg (0.127 mmol) [RuCl{(R)-segphos}]2(μ-Cl)3 [Me2NH2] were introduced in a nitrogen stream into a 1-L autoclave and flushed with hydrogen, and after introduction of hydrogen at a pressure of 1 MPa, the mixture was heated with stirring. The mixture was reacted at 90 to 95° C. for 7 hours. After the reaction solution was cooled to room temperature, the hydrogen was purged and replaced by nitrogen. The reaction solution was concentrated in a rotary evaporator and the residue was distilled under reduced pressure to give 263.3 g of the title compound (chemical purity, 96.2%; optical purity, 99.1% ee; and yield, 87%).
WORKUP
后处理
- customflushed with hydrogen
- temperatureafter introduction of hydrogen at a pressure of 1 MPa, the mixture was heated
- customThe mixture was reacted at 90 to 95° C. for 7 hours
- customthe hydrogen was purged
- concentrationThe reaction solution was concentrated in a rotary evaporator
- distillationthe residue was distilled under reduced pressure