反应详情

温度

80 °C

10 g of 2,2-Difluoro-2-pyridin-2-ylethyl 4-methylbenzenesulfonate (J) obtained in step 3, 5 g of NaI, 20 mL of DMSO and 90 mL of aqueous ammonia were taken in a 500 mL autoclave vessel. The reaction mixture was heated to 80° C. and a pressure of 15 to 17 kg of ammonia maintained for 30-40 hours. The volume of the reaction mass was reduced by vacuum distillation. The RM was washed with 60 mL of IPE. The pH of the RM was adjusted to 10-14 by adding a 50% NaOH solution and extracted three times with 60 mL of MDC. The combined MDC layers were washed with brine, dried over sodium sulphate and distilled under vacuum (crude weight=8 g). The crude mass obtained was dissolved with 10 mL of MDC, and to this 4.5 g benzene sulphonic acid (BSA) dissolved in 30 mL isopropyl acetate (IPAc) was added dropwise over a period of 30 minutes with stirring at RT. The RM was stirred for 30 minutes at RT. The solid obtained was filtered and washed with IPAc and dried under vacuum, resulting in 5 g of the titled compound (Yield=49.5%).

1. distillationThe volume of the reaction mass was reduced by vacuum distillation
2. washThe RM was washed with 60 mL of IPE
3. additionby adding a 50% NaOH solution
4. extractionextracted three times with 60 mL of MDC
5. washThe combined MDC layers were washed with brine
6. dry with materialdried over sodium sulphate
7. distillationdistilled under vacuum (crude weight=8 g)
8. customThe crude mass obtained
9. dissolutionwas dissolved with 10 mL of MDC
10. additionwas added dropwise over a period of 30 minutes
11. stirringThe RM was stirred for 30 minutes at RT
12. customThe solid obtained
13. filtrationwas filtered
14. washwashed with IPAc
15. customdried under vacuum