反应详情

温度

150 °C

To a solution of N-[1-({5-[(2-acetylhydrazino)carbonyl]-2-chlorophenyl}methyl)-1H-pyrazol-3-yl]-2,6-difluorobenzamide (for a preparation see Intermediate 51)(130 mg, 0.290 mmol) in THF (4 ml) was added 4A molecular sieves (513 mg) (pre-dried in an oven) and then (methoxycarbonylsulfamoyl)triethylammonium hydroxide, inner salt (21 mg, 0.088 mmol, Fluka). The reaction vessel was sealed and heated in a Biotage Initiator microwave to 150° C. for 25 min. The solvent was evaporated in vacuo, the residue was dissolved in methanol (1 ml) and then filtered through a hydrophobic frit. The filtrate was dissolved in DMSO (1 ml) and the sample was purified by MDAP on Sunfire C18 column using Acetonitrile-Water with a Formic acid modifier (Method B). The solvent was evaporated in vacuo to give the title compound as a white solid (13 mg); LCMS (System 3) MH+=430/432, tRET=2.54 min.

1. additionwas added
2. dry with material4A molecular sieves (513 mg) (pre-dried in an oven)
3. customThe reaction vessel was sealed
4. customThe solvent was evaporated in vacuo
5. dissolutionthe residue was dissolved in methanol (1 ml)
6. filtrationfiltered through a hydrophobic frit
7. dissolutionThe filtrate was dissolved in DMSO (1 ml)
8. customthe sample was purified by MDAP on Sunfire C18 column
9. customThe solvent was evaporated in vacuo