反应详情

Triethylamine (7.0 ml) was added dropwise to a solution of 3-hydroxy-6-methoxy-2,4,5-trimethylbenzyl chloride (10.73 g) and N-methyl-2-(2-isopropyl-5-methylphenoxy)ethylamine (10.37 g) in N,N-dimethylformamide (60 ml) while stirring the mixture at room temperature. Immediately after the dropwise addition, heat was developed and salt was precipitated. The mixture was stirred at room temperature for 2 hours and triethylamine (2.0 ml) was added. The mixture was stirred for 1 hour. The reaction mixture was poured on ice water and extracted with ethyl acetate to give a crude product. The product was purified by silica gel chromatography (eluent; ethyl acetate/benzene=1/1) to give 18.03 g of the title compound (pale brown solid).

1. additionImmediately after the dropwise addition
2. temperatureheat
3. customsalt was precipitated
4. stirringThe mixture was stirred at room temperature for 2 hours
5. additiontriethylamine (2.0 ml) was added
6. stirringThe mixture was stirred for 1 hour
7. additionThe reaction mixture was poured on ice water
8. extractionextracted with ethyl acetate
9. customto give a crude product
10. customThe product was purified by silica gel chromatography (eluent; ethyl acetate/benzene=1/1)