反应详情

A suspension of N′-(8-bromo-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carbonyl)-N′-isopropyl-hydrazinecarboxylic acid tert-butyl ester (6.14 g, 12.7 mmol) in methanol (49 mL) was treated with 4N HCl in dioxan (12.7 mL, 51.0 mmol) and stirred at RT for 0.75 h before being warmed to 50° C. and stirred for 3 h. The reaction mixture was concentrated in vacuo and the resultant solid was triturated with diethyl ether to give the title compound as a yellow brown solid (5.14 g, 12.3 mmol, 96%). LCMS: RT=4.79 min, [M+H]+=382/384.

1. temperaturebefore being warmed to 50° C.
2. stirringstirred for 3 h
3. concentrationThe reaction mixture was concentrated in vacuo
4. customthe resultant solid was triturated with diethyl ether