反应详情

温度

25 °C

3-Methyl-4-nitrobenzoic acid (5.525 mmol, 1.0 gram) was taken in a 25 mL two necked round bottom flask attached with a condenser, provided with a guard tube. To this, thionyl chloride (6.07 mmol, 0.735 gram) and 1,2-dichloroethane (5 mL) were added and the solution was refluxed for a period of 3 hours. This reaction mixture was added to another 100 mL flask, containing a solution of N-methylpiperazine (16.57 mmol, 1.66 grams) in 10 mL 1,2-dichloroethane, which is maintained at temperature below 5° C. The reaction mixture was then stirred for 0.5 hour at 25° C. After the completion of reaction, the reaction mixture was poured onto 50 mL water. 1,2-dichloroethane layer was separated, washed with water (2×10 mL), brine (10 mL) and dried over anhydrous sodium sulfate. The volatiles were removed under the reduced pressure to obtain thick syrupy mass. This thick syrupy mass was used for next step of reaction without purification.

1. customattached with a condenser
2. customprovided with a guard tube
3. temperaturethe solution was refluxed for a period of 3 hours
4. additionThis reaction mixture was added to another 100 mL flask
5. temperatureis maintained at temperature below 5° C
6. customAfter the completion of reaction
7. custom1,2-dichloroethane layer was separated
8. washwashed with water (2×10 mL), brine (10 mL)
9. dry with materialdried over anhydrous sodium sulfate
10. customThe volatiles were removed under the reduced pressure
11. customto obtain thick syrupy mass
12. customThis thick syrupy mass was used for next step of reaction without purification