HRID2116603
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
1.0 g (2.69 mmol) of 2-(ethyloxy)-2-oxoethyl 4-[(1-naphthalenyloxy)methyl]-1-piperidinecarboxylate, prepared in Step 7.3., is dissolved in 12 ml of a 7N solution of ammonia (84 mmol) in methanol. The solution is left to react at ambient temperature for 3 days. It is evaporated to dryness and the residue is purified by chromatography on silica gel, eluting with a 90/10 then 80/20, 70/30 and 50/50 mixture of dichloromethane and ethyl acetate and then with a 95/5 mixture of ethyl acetate and methanol. The eluate is subsequently recrystallized from ethyl acetate, to give 0.77 g of product.
WORKUP
后处理
- waitThe solution is left
- customto react at ambient temperature for 3 days
- customIt is evaporated to dryness
- customthe residue is purified by chromatography on silica gel
- washeluting with a 90/10
- addition80/20, 70/30 and 50/50 mixture of dichloromethane and ethyl acetate
- additionwith a 95/5 mixture of ethyl acetate and methanol
- customThe eluate is subsequently recrystallized from ethyl acetate