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 solution of [(1S)-1-(t-butyldiphenylsilyloxymethyl)-3-methylbutyl]carbamic acid benzyl ester (7.35 g, 15.0 mmol) (obtained as described in Reference Example 37(1)) in methanol (220 ml) was subjected to catalytic hydrogenation in the presence of 10% palladium on charcoal (7.35 g) at room temperature for 4 hours. After checking the completion of the reaction, the reaction mixture was filtered in order to remove the catalyst and the filtrate concentrated under reduced pressure. The residue was purified by chromatography on a silica gel column using methylene chloride:methanol (98:2→9:1) as the eluant to afford (1S)-1-(t-butyldiphenylsilyloxymethyl)-3-methylbutylamine (4.50 g, yield 84%) as a colorless oil.
WORKUP
后处理
- customthe completion of the reaction
- filtrationthe reaction mixture was filtered in order
- customto remove the catalyst
- concentrationthe filtrate concentrated under reduced pressure
- customThe residue was purified by chromatography on a silica gel column