反应详情

温度

120 °C

A glass microwave reaction vessel was charged with 5-(3-(6-chloropyrazin-2-yl)-1-tosyl-1H-indol-5-yl)-N-(4-methoxybenzyl)-1,3,4-thiadiazol-2-amine (400 mg, 0.663 mmol) in TFA (1.5 mL). The mixture was stirred and heated in a Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc., Uppsala, Sweden) at 120° C. for 15 min, then cooled to RT. The solvent was removed in vacuo and the residue was diluted with p-dioxane (2 mL) and aq. NaOH (5 M, 0.8 mL) and the mixture was heated in a microwave at 100° C. for 15 min. The mixture was cooled to RT, diluted with water and extracted with CHCl3/iPrOH (4:1). The combined organic layers were dried, filtered and concentrated to give the crude material. MS (ESI, pos. ion) m/z: 329 (M+1).

1. customA glass microwave reaction vessel
2. temperaturecooled to RT
3. customThe solvent was removed in vacuo
4. additionthe residue was diluted with p-dioxane (2 mL) and aq. NaOH (5 M, 0.8 mL)
5. temperaturethe mixture was heated in a microwave at 100° C. for 15 min
6. temperatureThe mixture was cooled to RT
7. additiondiluted with water
8. extractionextracted with CHCl3/iPrOH (4:1)
9. customThe combined organic layers were dried
10. filtrationfiltered
11. concentrationconcentrated