反应 #478516

反应方程式

6-bromo-2-naphthoic acid

ammonia

MeOH

→

title compound

收率 90.0%

6-bromo-2-naphthamide

收率 90.0%

溶剂

thionyl chloride

反应条件

后处理

1. 1
   浓缩After concentration in vacuo
2. 2
   workup.ADDITIONthe residue was rediluted in CH2Cl2
3. 3
   浓缩concentrated again
4. 4
   浓缩The mixture was then concentrated
5. 5
   过滤filtered
6. 6
   洗涤rinsed with AcOEt
7. 7
   干燥dried over MgSO4
8. 8
   过滤filtered
9. 9
   浓缩concentrated in vacuo

实验过程

6-bromo-2-naphthoic acid (2 g, 7.97 mmol) was stirred in thionyl chloride (13.28 ml) at 70° C. for 16 h. After concentration in vacuo, the residue was rediluted in CH2Cl2 and concentrated again. To the acid chloride intermediate was added ammonia in MeOH (7 M, 13.66 ml, 96 mmol) and the mixture was stirred at room temperature for 3 h. The mixture was then concentrated. The residue was taken up in AcOEt, filtered, rinsed with AcOEt and then dried over MgSO4, filtered and concentrated in vacuo. The title compound (1.802 g, 90%) was isolated as a beige solid. LC-MS (M+1) 251.9, t=1.34 min.

来源