反应 #448595

ord-13e1cd739e3b4ec59ea400f3adfb8c5f

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONafter addition
  2. 2
    洗涤was then washed with water (50 ml)
  3. 3
    干燥The organic phase was dried (MgSO4) and volatile material
  4. 4
    其他was removed by evaporation
  5. 5
    其他to give a yellow oil
  6. 6
    其他The oil was purified by elution with dichloromethane through a silica gel Mega Bond Elut column

实验过程

A solution of bromine (0.11 ml) in chloroform (20 ml) was added dropwise over 20 minutes to a solution of 2-amino-5-methylpyrazine (0.218 g) in chloroform (30 ml) which was protected from light. The reaction mixture was stirred for 90 minutes after addition was complete and was then washed with water (50 ml). The organic phase was dried (MgSO4) and volatile material was removed by evaporation to give a yellow oil. The oil was purified by elution with dichloromethane through a silica gel Mega Bond Elut column to give 2-amino-3-bromo-5-methylpyrazine (0.286 g) as a white solid, m.p. 51°-52° C.; mass spectrum (+ve CI): 188 (M+H)+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05866568uspto-grants-1999_02