反应详情

A mechanically stirred mixture of 310 g (0.73 mol) of 1,4-dichloro-5-[(2,4,6-trimethylphenyl)methoxy]-9,10-anthracenedione, 260 g (2.19 mol) of 2-[(2-hydrazinoethyl)amino]ethanol, 381 ml (2.19 mol) of N,N-diisopropylethylamine, and 4.8 l of acetonitrile was heated at reflux for 22 hr. The cooled mixture was concentrated in vacuo to leave a residue, showing a ~1:4 ratio of 12:13, that was triturated with water. The solids were collected by filtration, washed with methanol, and dried at 220 mm/50° C./18 hr to leave 237 g (66%) of crude 13, mp 147°-158° C.

1. temperaturewas heated
2. temperatureat reflux for 22 hr
3. concentrationThe cooled mixture was concentrated in vacuo
4. customto leave a residue
5. customthat was triturated with water
6. filtrationThe solids were collected by filtration
7. washwashed with methanol
8. customdried at 220 mm/50° C./18 hr
9. customto leave 237 g (66%) of crude 13, mp 147°-158° C.