反应 #2320172

反应方程式

4-bromo-6-methoxy-[1,5]naphthyridin-3-ylamine

nitrosonium tetrafluoroborate

→

title compound

收率 90.0%

4-Bromo-6-methoxy-[1,5]naphthyridine-3-diazonium tetrafluoroborate

收率 90.0%

溶剂

THF

反应条件

后处理

1. 1
   workup.ADDITIONwas added portion-wise over 30 min (approximately 2 g portions)
2. 2
   过滤The orange solid was collected by suction filtration
3. 3
   洗涤washed with ice-cold THF
4. 4
   其他dried under vacuum

实验过程

A solution of 4-bromo-6-methoxy-[1,5]naphthyridin-3-ylamine (25.2 g, 99.2 mmol) in dry THF (400 mL) was maintained at −5° C. while nitrosonium tetrafluoroborate (12.9 g, 110 mmol) was added portion-wise over 30 min (approximately 2 g portions). The reaction was continued for an additional 1 h at −5° C., at which time TLC* and LC/MS indicated that the reaction was complete. The orange solid was collected by suction filtration, washed with ice-cold THF and dried under vacuum to provide the title compound (31.42 g, 90%).

来源