反应 #9443

反应方程式

7-bromoquinolin-4-ol

Nitric acid

nitric acid

→

7-bromo-3-nitro-quinolin-4-ol

收率 78.1%

溶剂

propionic acid

propionic acid

反应条件

后处理

1. 1
   其他was brought to 110° C
2. 2
   温度was maintained between 110–115° C
3. 3
   workup.ADDITIONUpon complete addition
4. 4
   workup.STIRRINGthe reaction was stirred for 1 h at 110° C.
5. 5
   过滤the solid was collected by filtration
6. 6
   洗涤The filter cake was washed with ice cold ethanol until the washings
7. 7
   其他the product was dried at 60° C. under vacuum

实验过程

A stirred suspension of 7-bromoquinolin-4-ol (162 g, 0.723 mol) in propionic acid (1500 mL) was brought to 110° C. 70% Nitric acid (85 g) was added dropwise over 1 h such that the temperature was maintained between 110–115° C. After half of the nitric acid had been added, stirring became difficult due to the formation of solids and an additional 200 mL of propionic acid was added. Upon complete addition, the reaction was stirred for 1 h at 110° C., cooled to room temperature, and the solid was collected by filtration. The filter cake was washed with ice cold ethanol until the washings were nearly colorless (800 mL), and the product was dried at 60° C. under vacuum to afford 152 g of 7-bromo-3-nitro-quinolin-4-ol as a pale yellow solid.

来源