反应详情

温度

20 °C

3-Aminophenylacetic acid (1 wt) was suspended in methanol (5 vol) under nitrogen at 20° C. Chlorotrimethylsilane (1.26 vol) was added over 60 minutes at 20° C. The reaction mixture was stirred at 20° C. for one hour, then concentrated under reduced pressure to 3 vol. Methyl-t-butyl ether (4 vol) was added and the resulting suspension was stirred at room temperature for 18 hours. The solid was collected by filtration, washing with methyl-t-butyl ether (4×1 vol). The material was dried in oven at 40° C. for 5 hours to give the title compound.

1. concentrationconcentrated under reduced pressure to 3 vol. Methyl-t-butyl ether (4 vol)
2. additionwas added
3. stirringthe resulting suspension was stirred at room temperature for 18 hours
4. filtrationThe solid was collected by filtration
5. washwashing with methyl-t-butyl ether (4×1 vol)
6. customThe material was dried in oven at 40° C. for 5 hours