反应详情

Two hundred mg (0.62 mM) of 6-carbethoxyaminobenzothieno[3,2-h]isoquinoline (9), prepared in the preceding Example, was added to a solution of 2 g KOH in 5 ml ethanol and 2 ml water. Two layers formed. The mixture was stirred and heated at reflux for approximately 2-3 hr. A yellow solid separated after about an hour, and was collected via filtration and air dried to give 160 mg product, m.p. 220° C.-225° C. This initial product was recrystallized twice from a mixture of DMF and water to provide 120 mg final product, m.p. 223.5° C.-224.5° C., which was then characterized via I.R. and mass spectrometry as compound 10.

1. customTwo layers formed
2. temperatureheated
3. temperatureat reflux for approximately 2-3 hr
4. customA yellow solid separated after about an hour
5. filtrationwas collected via filtration and air
6. customdried