反应详情

20.8 g of LiOH.H2O are added at 0° C. to a solution of 24.5 g of 2,2-difluoro-4-amino-1,3-benzodioxole in 70 ml of dimethyl sulfoxide. The mixture is then stirred for 20 minutes. Subsequently, a solution of 38.3 g of 2,4-dinitro-6-trifluoromethylchlorobenzene in 70 ml of dimethyl sulfoxide is added, and the resultant reaction mixture is stirred at 0° C. for 20 minutes and then heated to room temperature. After 5 hours, the mixture is poured into 350 ml of water, acidified with dilute hydrochloric acid and extracted several times with diethyl ether. The combined ether phases are washed three times with a 5 % solution of sodium carbonate and then with 5 % hydrochloric acid and dried over sodium sulfate, and the solvent is evaporated off in vacuo. The residue comprises 51.6 g of orangebrown crystals which are recrystallised in toluene. Yield: 41.6 g; melting point: 144°-146° C.

1. customthe resultant reaction mixture
2. stirringis stirred at 0° C. for 20 minutes
3. waitAfter 5 hours
4. extractionextracted several times with diethyl ether
5. washThe combined ether phases are washed three times with a 5 % solution of sodium carbonate
6. dry with materialwith 5 % hydrochloric acid and dried over sodium sulfate
7. customthe solvent is evaporated off in vacuo
8. customare recrystallised in toluene