反应详情

温度

80 °C

2-(Toluene-4-sulfonylamino)-benzoic acid methyl ester from Example E5.1 (100 g) was dissolved in DMF (250 ml). Potassium carbonate (125 g) and ethyl 4-bromobutanoate (60 g) were added and the mixture was heated at 80° C. for 18 h. The mixture was cooled to room temperature, filtered and reduced in vacuo. The residue was partitioned between chloroform and 1M HCl solution. The aqueous layer was extracted with chloroform. The organic layers were combined, washed with brine, dried, filtered and concentrated in vacuo. The material was crystallised from EtOAc/hexane and dried in a vacuum oven at 60° C. for 3 hours to yield the title compound (98.6 g, 72%).

1. temperatureThe mixture was cooled to room temperature
2. filtrationfiltered
3. customThe residue was partitioned between chloroform and 1M HCl solution
4. extractionThe aqueous layer was extracted with chloroform
5. washwashed with brine
6. customdried
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe material was crystallised from EtOAc/hexane
10. customdried in a vacuum oven at 60° C. for 3 hours