反应详情

Concentrated hydrochloric acid (0.1 mL) was added to 1-(3-methoxymethoxy-phenyl)-2-methylamino-ethanol (300 mg, 1.42 mmol) dissolved in methanol (3 mL). The resulting mixture was heated at reflux for about 30 minutes, and then cooled to ambient temperature. The mixture was concentrated to dryness, and the residue was purified by flash column chromatography on silica gel (1×16 cm, dichloromethane/methanol/ammonium hydroxide=45/8/1 elution) to give the title compound (160 mg, 67%). 1H NMR (300 MHz, CD3OD) δ 7.14 (t, 1H, J=8.1 Hz), 6.81-6.80 (m, 2H), 6.69-6.66 (m, 1H), 4.71-4.67 (m, 1H), 2.78-2.66 (m, 2H), 2.41 (s, 3H); LC-MS: m/z=168 (MH)+; HPLC: 98% (Purity).

1. temperatureThe resulting mixture was heated
2. temperatureat reflux for about 30 minutes
3. concentrationThe mixture was concentrated to dryness
4. customthe residue was purified by flash column chromatography on silica gel (1×16 cm, dichloromethane/methanol/ammonium hydroxide=45/8/1 elution)