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
The title compound was prepared in the same way as described by M. Lemaire, F. Posada, J.-G. Gourcy and G. Jeminet, Synlett, 1995, 627. A solution of (R)-(2,2-dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate (3.9 g, 18.55 mmol) and benzylamine (8.10 ml, 74.2 mmol) was refluxed in CH3CN (50 ml) for 48 h. The solvent was evaporated and the residue dissolved in EtOAc and washed with aqueous sat. NaHCO3, dried and the solvent evaporated. The residue was chromatographed (EtOAc-hex, 6:4 then 8:2) to give (S)—N-benzyl-1-(2,2-dimethyl-1,3-dioxolan-4-yl)methanamine (3.1 g, 14.01 mmol, 76% yield) as a yellow oil. [α]D21 +4.3 (c, 0.69, CHCl3). The 1H NMR and 13C NMR were identical to that of compound 3.2.
WORKUP
后处理
- customThe title compound was prepared in the same way
- customThe solvent was evaporated
- dissolutionthe residue dissolved in EtOAc
- washwashed with aqueous sat. NaHCO3
- customdried
- customthe solvent evaporated
- customThe residue was chromatographed (EtOAc-hex, 6:4