反应详情

温度

100 °C

To 4-amino-2-methylphenol (Aldrich, 5.0 g, 40.6 mmol) was added 6M HCl (100 mL) and heated to 100° C. with stirring. Toluene (30 mL) was added, followed with the slow addition of crotonaldehyde (6.7 mL, 81.2 mmol) at 100° C. The mixture was stirred at 100° C. for 2 additional hours, cooled to room temperature. The water layer was separated, neutralized by NaHCO3 solution. The solid formed was filtered and collected. LCMS-ESI+ (m/z): [M+H]+ calc'd for C11H12NO: 174.2; Found: 174.2.

1. stirringThe mixture was stirred at 100° C. for 2 additional hours
2. temperaturecooled to room temperature
3. customThe water layer was separated
4. customThe solid formed
5. filtrationwas filtered
6. customcollected