HRID5650
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
Under nitrogen atmosphere and stirring, a MeOH solution (15 ml) of g 0.85 of (+)2-ethylthiomethyl-3-carboethoxy-5-carbomethoxy-4-(3-chlorophenyl)-6-methyl-1,4-dihydropyridine, cooled at 30° C. is treated with NaH2PO4 (g 1.45) and with Na/Hg amalgam (2.64 g) (10% in Na). After 15 minutes the solution is filtered and evaporated to a small volume under vacuum. The residue is partitioned between water (ml 20) and AcOEt (3×30 ml), the organic phases are collected to give after the usual work-up 0.56 g of (+)-2,6-dimethyl-4-(3-chlorophenyl)-3-carboethoxy-5-carbomethoxy-1,4-dihydropyridine [α]D =+5.5°; c=4.1 CH2Cl2.
WORKUP
后处理
- filtrationAfter 15 minutes the solution is filtered
- customevaporated to a small volume under vacuum
- customThe residue is partitioned between water (ml 20) and AcOEt (3×30 ml)
- customthe organic phases are collected