HRID2236545

反应详情

EQUATION

反应方程式

HRID 2236545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of chloro-(4-methoxy-5-nitro-pyridin-2-yl)-acetic acid tert-butyl ester (2.98 g, 9.84 mole) and acetic acid (25 mL) is refluxed for 6 hours, cooled and evaporated. The residue is dissolved in dichloromethane, passed thru a pad of magnesol, evaporated to dryness and crystallized from 3:1 hexanes/ethyl acetate to give a light yellow solid, 1.78 g, (89%); MS (ES+): m/z 203.2, 205.2 (M+H).

WORKUP

后处理

  1. temperatureis refluxed for 6 hours
  2. temperaturecooled
  3. customevaporated
  4. dissolutionThe residue is dissolved in dichloromethane
  5. customevaporated to dryness
  6. customcrystallized from 3:1 hexanes/ethyl acetate
  7. customto give a light yellow solid, 1.78 g, (89%)