反应 #78855

ord-0326d4b48151442e9091b15321845211

反应方程式

Clc1cnccn1
2-chloropyrazine
[H-].[Na+]
Sodium hydride
O=Cc1c[nH]cn1
1H-imidazole-4-carboxaldehyde
O=Cc1cn(-c2cnccn2)cn1
title compound
收率 99.4%
O=Cc1cn(-c2cnccn2)cn1
1-(2-pyrazinyl)-1H-imidazole-4-carboxaldehyde
收率 99.4%

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度to warm to RT
  2. 2
    温度The resulting mixture was heated to 100° C. for 18 h
  3. 3
    其他The solvent was evaporated
  4. 4
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  5. 5
    洗涤washed with water and brine
  6. 6
    干燥dried (MgSO4)
  7. 7
    浓缩concentrated

实验过程

Sodium hydride (60% in oil, 720 mg, 18.0 mmol) was added to a 0° C. solution of 1H-imidazole-4-carboxaldehyde (2.20 g, 18.0 mmol) in DMF (8 mL). After stirring for 20 min at 0° C., the mixture was allowed to warm to RT and a solution of 2-chloropyrazine (2.06 g, 17.9 mmol) in DMF (4 mL) was added. The resulting mixture was heated to 100° C. for 18 h. The solvent was evaporated, the residue was dissolved in ethyl acetate, washed with water and brine, dried (MgSO4), and concentrated to provide 3.10 g (86%) of the title compound. MS 175 (M+H)+

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06713455B2uspto-grants-2004_03