反应详情

A stirring suspension of tert-butyl 2-(2-(2-(benzyloxy)-3,3,3-trifluoro-2-methylpropanoyl)hydrazine carbonyl)-6-methoxy-5-(trifluoromethyl)pyridin-3-ylcarbamate (step 1) (1 g, 1.723 mmol) in dry THF (20 ml) was treated with Burgess reagent (3 equiv.) and heated at reflux under N2 for 1 h 45 min. The RM was reduced in vacuo to approximate volume of 5 ml and diluted with EtOAc (150 ml). The mixture was washed with 2M NaOH, 0.5M HCl, water, brine and dried (MgSO4) and concentrated in vacuo. The crude product was triturated with MeOH to afford the title compound. LC-MS Rt=1.59 min [M+H]+ 563.5 Method High pH_v003.

1. temperatureheated
2. temperatureat reflux under N2 for 1 h 45 min
3. washThe mixture was washed with 2M NaOH, 0.5M HCl, water, brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe crude product was triturated with MeOH