反应详情

N-(2-chloroethyl)benzamide (2.1 g, 11.2 mmol), PCl5 (3.5 g, 16.8 mmol) were dissolved in m-Xylene (100 mL) and refluxed for 2 h. After cooling down the reaction flask to room temperature, 2,4-diisopropyldibenzo[b,d]furan-1-amine (3.3 g, 12.3 mmol) was added to it and the reaction mixture was refluxed overnight. From the cooled reaction mixture white precipitate was filtered out. Precipitate was dissolved in ethylacetate and partitioned between ethylacetate and aqueous Na2CO3. Organic phase was extracted out and dried under vacuum. Target compound (4 g, 90% yield) was used in next step without further purification.

1. temperaturerefluxed for 2 h
2. temperaturethe reaction mixture was refluxed overnight
3. customFrom the cooled reaction mixture white precipitate
4. filtrationwas filtered out
5. dissolutionPrecipitate was dissolved in ethylacetate
6. custompartitioned between ethylacetate and aqueous Na2CO3
7. extractionOrganic phase was extracted out
8. customdried under vacuum