反应详情

温度

79.5 °C

Combine (S)-7-chloro-10-[3-(2-methoxy-ethyl)-4-methyl-piperazin-1-yl]-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene (39.7 g, 97.6 mmol) and 2-propanol (IPA, 397 mL) at ambient temperature and hear to 80-81° C. Add a solution of concentrated HCl (17.1 mL, 206 mmol) in IPA (79 mL) over 20-30 minutes. Maintain the temperature of the resulting mixture at 79-80° C. for 1.5 hours. Shut heat source and allow the mixture to cool slowly to 30° C. over 3 hours. Cool to 0-5° C. and stir for an additional hour. Filter the solids and rinse with ice cold IPA (3×50 mL). Dry at 50° C. to afford 46.5 g (99.3%) of the title compound. KF analysis gives 5.47% H2O, Chloride analysis affords a value of 12.8%.

1. customat ambient temperature
2. customhear to 80-81° C
3. temperatureShut heat source
4. temperatureto cool slowly to 30° C. over 3 hours
5. temperatureCool to 0-5° C.
6. filtrationFilter the solids
7. washrinse with ice cold IPA (3×50 mL)
8. customDry at 50° C.