反应详情

A 3 L 3-necked flask is equipped with a condenser, argon inlet, thermowell, magnetic stirrer. The flask is purged with argon then charged with 2,3,4,5-tetramethylbenzoic acid (138.3 g, 0.776 mol), methylene chloride (1.5 L), thionyl chloride (73.5 mL, 1.01 mol) and N, N-dimethylformamide (2.0 mL, 0.026 mol). The resulting suspension is heated to reflux, after a clear solution is formed, heating is continued for 3.5 hours. The solution is allowed to cool then concentrated in vacuo. Last traces of thionyl chloride are removed by co-distillation with toluene (2×100 mL). The remaining oil is dried under high vacuum then used without further purification. Additional reactions are carded out to produce a total of 218 g of 2,3,4,5-tetramethylbenzoyl chloride.

1. customA 3 L 3-necked flask is equipped with a condenser, argon inlet
2. customThe flask is purged with argon
3. temperatureThe resulting suspension is heated
4. temperatureto reflux
5. customafter a clear solution is formed
6. temperatureheating
7. temperatureto cool
8. concentrationthen concentrated in vacuo
9. customLast traces of thionyl chloride are removed by co-distillation with toluene (2×100 mL)
10. customThe remaining oil is dried under high vacuum
11. customthen used without further purification