methyl 3-amino-3-sulfanylidenepropanoate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of the compound (107 mg, 0.30 mmol) obtained in step 5 and methyl 3-amino-3-thioxopropanoate (48.7 mg, 0.37 mmol) in EtOH (3 mL) was stirred at 90° C. for 14 hr. The reaction mixture was concentrated under reduced pressure, and the residue was purified by NH-silica gel column chromatography (solvent gradient; 5→80% ethyl acetate/hexane) to give a crude product ethyl 2-(4-(1-tert-butyl-5-(4-methoxyphenyl)-1H-pyrazol-4-yl)thiazol-2-yl)acetate as a colorless oil, which was used for the next step without purification. The reaction mixture was concentrated under reduced pressure the residue was purified by NH-silica gel column chromatography (solvent gradient; 5→80% ethyl acetate/hexane)