反应详情

温度

131 °C

D8 (86 mg), 3-bromopropionate (52 mg), Cs2CO3 (126 mg) and DMF (1 ml) were placed in a microwave vial and stirred at 131° C. in the microwave reactor for 1.5 hours. The reaction mixture was then evaporated to dryness and treated with 2M aq. NaOH and EtOH (20 ml). This solution was stirred at 50° C. for 4 hours and then neutralised with HCl and evaporated to remove the EtOH. The aqueous solution was then extracted twice with EtOAc and the combined extracts evaporated. The residue was dissolved in DMSO, filtered, treated with MeCN causing precipitation of the product which was filtered and washed with MeCN to give the title compound (23 mg) as an off-white solid. δH (d6-DMSO, 400 MHz): 2.47-2.57 (solvent+2H) 4.37 (2H, t), 7.51-7.59 (5H, m), 7.72 (1H, s), 7.76 (1H, d), 7.89 (1H, d), 8.17 (1H, s), 8.25 (1H, s). MS (ES): C24H16ClF3N3O2S requires 517; found 516 (M−H+).

1. customThe reaction mixture was then evaporated to dryness
2. additiontreated with 2M aq. NaOH and EtOH (20 ml)
3. stirringThis solution was stirred at 50° C. for 4 hours
4. customevaporated
5. customto remove the EtOH
6. extractionThe aqueous solution was then extracted twice with EtOAc
7. customthe combined extracts evaporated
8. dissolutionThe residue was dissolved in DMSO
9. filtrationfiltered
10. additiontreated with MeCN causing precipitation of the product which
11. filtrationwas filtered
12. washwashed with MeCN