反应详情

A mixture of 4-amino-8-bromo-6-nitro-quinazolin-2-ol (24.1 mg, 0.0845 mmol), sulfamic acid (16.4 mg, 0.169 mmol) and 1-(3-aminopropyl)-4-methylpiperazine (1 ml) was heated at reflux for 7 h. The cooled reaction mixture was poured into 10 ml ice water. The resulting precipitate was collected and purified by preparative HPLC. 19.2 mg product was obtained. Yield: 40%; 1H NMR (500 MHz, DMSO-d6): δ 1.91521–1.95482 (m, 2H), 2.78103(s, 8H), 3.16555(b, 4H), 8.68221–8.68666(d, J=2.225 Hz, 1H), 9.10824–9.11291(d, J=2.335 Hz, 1H); ESI-MS: 425, 427 (M++1)

1. temperaturewas heated
2. temperatureat reflux for 7 h
3. customThe cooled reaction mixture
4. customThe resulting precipitate was collected
5. custompurified by preparative HPLC