反应详情

温度

50 °C

A solution of N-(4-morpholinophenyl)-8-amino-5-methoxy-1,2,3,4-tetrahydronaphthalene-2-carboxamide (1.4 g, 3.5 mmol), bis (2-chloroethyl)-methylamine hydrochloride (960 mg, 5 mmol) and sodium hydrogen carbonate (420 mg, 5 mmol) in n-butanol (30 mL) was heated at 90° C. for 5 h. After cooling, 2 M ammonium hydroxide (30 mIL) was added and the mixture heated at 50° C. for 1 h. The phases were separated, evaporated in vacuo and purified by flash chromatography on a silica gel column with chloroforrn/ethanol/conc. ammonium hydroxide 90/10/0.3 as eluent. Yield: 320 mg (20 %) of the title compound: mp 230-232° C.; EIMS (70 eV) m/z (relative intensity) 464 (75, M+).

1. temperatureAfter cooling
2. customThe phases were separated
3. customevaporated in vacuo
4. custompurified by flash chromatography on a silica gel column with chloroforrn/ethanol/conc