HRID69617

反应详情

EQUATION

反应方程式

HRID 69617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 6-chloro-5-nitronicotinate (2.0 g, 9.23 mmol) was added to methyl piperidine-2-carboxylate (5.2 g, 36.92 mmol) while stirring at room temperature. The viscous yellow reaction was heated to 90° C. for one h and then allowed to cool back to room temperature. The reaction was diluted with dichloromethane (20 mL) and purified via column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes) to yield the title compound (2.95 g, 99% yield) as a yellow oil. [M+H] calc'd for C14H17N3O6, 324; found, 324.

WORKUP

后处理

  1. customThe viscous yellow reaction
  2. temperaturewas heated to 90° C. for one h
  3. temperatureto cool back to room temperature
  4. custompurified via column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes)