反应详情

温度

40 °C

To a 40° C. warm mixture of 10.0 g (28.6 mmol) 3-[2-(4-methylphenylsulphonylamino)-ethyl]-phenoxyacetic acid and 100 ml abs. THF one adds 4.64 g (28.6 mmol) carbonyl-bisimidazole and allows to react for 10 min. 0.4 g (28.6 mmol) p-nitrophenol are then added thereto. After 10 min. one adds thereto 3.1 g (28.6 mmol) benzylamine and stirs fortwo hrs. at 60° C. Subsequently, THF is distilled off, the residue mixed with ice and dil. HCl and shaken out with methylene chloride. One extracts the organic phase twice with NaHCO3 solution and once with water. After drying with MgSO4, it is evaporated and recrystallised (ethanol). Yield 10.2 g (81% of theory); m.p. 118°-120° C.

1. customto react for 10 min
2. additionAfter 10 min. one adds
3. customat 60° C
4. distillationSubsequently, THF is distilled off
5. additionthe residue mixed with ice and dil. HCl
6. dry with materialAfter drying with MgSO4, it
7. customis evaporated
8. customrecrystallised (ethanol)