反应详情

0.50 g (1.94 mmol) ethyl 3-chloro-4-(2-hydroxy-1-methyl-ethylamino)-benzoate are placed in 30 ml THF together with 0.22 g (2.20 mmol) triethylamine and 1.10 ml (2.08 mmol) 20% phosgene solution in toluene is added with stirring at ambient temperature. The mixture is stirred for 1 hour at ambient temperature, then 1 ml of water is added and the mixture is stirred for another 10 minutes. The mixture is then evaporated down i. vac., combined with water and extracted with ethyl acetate. The combined organic phases are washed with water and sat. sodium chloride solution, dried over sodium sulphate and evaporated down i. vac.

1. additionis added
2. stirringThe mixture is stirred for 1 hour at ambient temperature
3. stirringthe mixture is stirred for another 10 minutes
4. customThe mixture is then evaporated down i
5. extractionextracted with ethyl acetate
6. washThe combined organic phases are washed with water and sat. sodium chloride solution
7. dry with materialdried over sodium sulphate
8. customevaporated down i