HRID10193
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
A mixture of 1 g (4.3 mmole)(4S,5S)-5-(4-tert-butylphenyl)-4-methyl-oxazolidin-2-one p(see preparation 4, step 2), 2 g (31.74 mmole) ammonium formate and 0.1 g 10% palladium on carbon in 25 mL methanol was heated under reflux for 2 hrs. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was partitioned between 10 mL 10% sodium carbonate and 25 mL ethyl acetate. The organic phase was dried (magnesium sulfate) and concentrated under reduced pressure. The title compound was isolated as the hydrochloride salt from diethyl ether, 0.93 g (95%), m.p.259.5–261.3° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 2 hrs
- filtrationThe mixture was filtered
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was partitioned between 10 mL 10% sodium carbonate and 25 mL ethyl acetate
- dry with materialThe organic phase was dried (magnesium sulfate)
- concentrationconcentrated under reduced pressure