HRID1653647

反应详情

EQUATION

反应方程式

HRID 1653647 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a methanol (80 ml) suspension of 7 g (24.6 mmol) of methyl 6-azido-3-benzyloxypicolinate in a 200 ml round bottomed flask, 1 g of palladium carbon (10%) was added under a nitrogen gas stream, and 7.8 g (123 mmol) of ammonium formate was further added thereto. The mixture was stirred at room temperature for 12 hours. The catalyst was filtered off, and the filtrate was concentrated and dissolved in chloroform. The solvent was washed with water, dried and concentrated. Crystals thereby formed were collected by filtration and washed with diisopropyl ether to obtain 3.57 g (yield: 86.3%) of methyl 6-amino-3-hydroxypicolinate.

WORKUP

后处理

  1. additionwas further added
  2. filtrationThe catalyst was filtered off
  3. concentrationthe filtrate was concentrated
  4. dissolutiondissolved in chloroform
  5. washThe solvent was washed with water
  6. customdried
  7. concentrationconcentrated
  8. customCrystals thereby formed
  9. filtrationwere collected by filtration
  10. washwashed with diisopropyl ether