반응 #9443

반응 방정식

7-bromoquinolin-4-ol

Nitric acid

nitric acid

→

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

수율 78.1%

용매

propionic acid

propionic acid

반응 조건

후처리

1. 1
   기타was brought to 110° C
2. 2
   온도was 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
   여과the solid was collected by filtration
6. 6
   세척The filter cake was washed with ice cold ethanol until the washings
7. 7
   기타the product was dried at 60° C. under vacuum

실험 절차

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.

출처