HRID78726

反应详情

EQUATION

反应方程式

HRID 78726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Methyl 3-amino-6-bromopyrazine-2-carboxylate (15 g, 64.6 mmol) was suspended in 150 mL of dioxane at room temperature. Hydrazine hydrate (6.5 g, 130 mmol) was added and the reaction mixture was stirred at 60° C. for 2 hours. Initially the mixture became clear, but after a while a precipitate formed. The mixture was cooled to ambient temperature and crude product filtered off. The solid was washed with TBME and subsequently stirred in water. The material was filtered and washed with acetone to afford 3-Amino-6-bromopyrazine-2-carbohydrazide 4 as slightly yellow solid. The material was dried in vacuo. (10.5 g, 70%).

WORKUP

后处理

  1. customafter a while a precipitate formed
  2. temperatureThe mixture was cooled to ambient temperature
  3. filtrationcrude product filtered off
  4. washThe solid was washed with TBME
  5. stirringsubsequently stirred in water
  6. filtrationThe material was filtered
  7. washwashed with acetone