反应详情

1-Chloro-N,N,2-trimethyl-1-propenylamine (0.13 mL, 1.01 mmol) was added to a solution of 3-[(2-methyl-1,1-dioxido-3,4-dihydro-2H-5,1,2-benzoxathiazepin-7-yl)oxy]-5-{[(1S)-1-methyl-2-(methyloxy)ethyl]oxy}benzoic acid (0.22 g, 0.50 mmol) in DCM (8 mL) and stirred for 1 hour. 1,1-Dimethylethyl 3-amino-1H-pyrazole-1-carboxylate (231 mg, 1.26 mmol) then pyridine (0.1 mL, 1.26 mmol) were added and the reaction stirred until the reaction was complete. The reaction mixture was reduced in vacuo and ethyl acetate (50 mL) and water (50 mL) were added. The aqueous layer was further extracted into ethyl acetate (50 mL) and the combined organics washed with water (50 mL), brine (50 mL), dried (MgSO4), filtered and reduced in vacuo to give a golden oil which was chromatographed on silica, eluting with 25-70% ethyl acetate in isohexane then 0-5% methanol in DCM, to give the desired compound as a colourless oil (50 mg).

1. stirringthe reaction stirred until the reaction
2. additionwere added
3. extractionThe aqueous layer was further extracted into ethyl acetate (50 mL)
4. washthe combined organics washed with water (50 mL), brine (50 mL)
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customto give a golden oil which
8. customwas chromatographed on silica
9. washeluting with 25-70% ethyl acetate in isohexane