反应详情

温度

20 °C

2-Iodo-4-(1-methylethyl)phenol (13.1 g., 0.05 mole) is dissolved in a mixture of acetic acid (50 ml.) and 96% sulfuric acid (5 ml.) and powdered 2-chloro-N-(hydroxymethyl)acetamide (6.15 g., 0.05 mole) is added during 10 minutes with stirring at 20° C. The solution is stirred for 2.5 hours and then added to 300 ml. of water. The crude solid (18 g.) is collected and refluxed in ethanol (25 ml.)-hydrochloric acid (10 ml.) for 2 hours. The solid (7.5 g.) that separates on cooling, namely 2-aminomethyl-4-(1-methylethyl)-6-iodophenol hydrochloride, is purified by crystallization from ethanol 12N-hydrochloric acid (7:3) to obtain 2-aminomethyl-4-(1-methylethyl)-6-iodophenol hydrochloride (7 g.), m.p. 211°-212° C. (dec.).

1. additionis added during 10 minutes
2. stirringThe solution is stirred for 2.5 hours
3. additionadded to 300 ml
4. customThe crude solid (18 g.) is collected
5. temperaturerefluxed in ethanol (25 ml.)-hydrochloric acid (10 ml.) for 2 hours
6. temperatureon cooling
7. customnamely 2-aminomethyl-4-(1-methylethyl)-6-iodophenol hydrochloride, is purified by crystallization from ethanol 12N-hydrochloric acid (7:3)