HRID2116603

反应详情

EQUATION

反应方程式

HRID 2116603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. waitThe solution is left
  2. customto react at ambient temperature for 3 days
  3. customIt is evaporated to dryness
  4. customthe residue is purified by chromatography on silica gel
  5. washeluting with a 90/10
  6. addition80/20, 70/30 and 50/50 mixture of dichloromethane and ethyl acetate
  7. additionwith a 95/5 mixture of ethyl acetate and methanol
  8. customThe eluate is subsequently recrystallized from ethyl acetate