反应详情

温度

-10 °C

The flask containing the SOCl2/H2O solution is cooled again to −10° C. and a catalytic amount of Cu(I)Cl (˜50 mg) was added. The solution turns dark green in color. The flask was fitted with a 500 mL addition funnel (previously chilled to 0° C.) and the 3,4,5-trifluorodiazobenzene solution was quickly transferred to the funnel. The solution was immediately added dropwise over a period of 3 min. After addition, the reaction mixture slowly turns darker green in color, but after stirring for 5 min becomes bright, lime green. The reaction was stirred for an additional hour while warming to room temperature. The reaction mixture was transferred to a separatory funnel and extracted with CH2Cl2 (3×200 mL). The organic phases are combined and dried over anhydrous Na2SO4, filtered, and concentrated to give a dark-bronze oil (79.5 g, 83%).

1. customThe flask was fitted with a 500 mL addition funnel (
2. additionThe solution was immediately added dropwise over a period of 3 min
3. additionAfter addition
4. stirringThe reaction was stirred for an additional hour
5. temperaturewhile warming to room temperature
6. customThe reaction mixture was transferred to a separatory funnel
7. extractionextracted with CH2Cl2 (3×200 mL)
8. dry with materialdried over anhydrous Na2SO4
9. filtrationfiltered
10. concentrationconcentrated