HRID1527730

反应详情

EQUATION

反应方程式

HRID 1527730 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

A mixture of 2-((3-fluoro-4-nitrophenoxy)methyl)-5-methylpyridine (2.0 g, 7.6 mmol), 4-bromobenzyl amine (1.6 g, 8.4 mmol), DIPEA (2.63 mL, 15.3 mmol) and acetonitrile (25.4 mL) were sealed in a reaction vessel and heated to 60° Celsius for 24 h. The mixture was cooled to RT, transferred to a round bottomed flask and concentrated to dryness. The crude mixture was heated to 70° Celsius in a minimum amount of i-PrOH until homogeneous and cooled to RT. The resulting mixture was filtered to collect the yellow solids which were dried to afford the title compound (2.82 g, 86%). MS (ESI): mass calcd. for C20H18BrN3O3, 427.053; m/z found, 428.0 [M+H]+.

WORKUP

后处理

  1. customwere sealed in a reaction vessel
  2. temperatureThe mixture was cooled to RT
  3. customtransferred to a round bottomed flask
  4. concentrationconcentrated to dryness
  5. temperatureThe crude mixture was heated to 70° Celsius in a minimum amount of i-PrOH until homogeneous and
  6. temperaturecooled to RT
  7. filtrationThe resulting mixture was filtered
  8. customto collect the yellow solids which
  9. customwere dried