反应详情

3.10 g (19.1 mmol) 5-chloro-thiophene-2-carboxylic acid are combined with 4.44 ml (40 mmol) NMM and 6.42 g (20 mmol) TBTU in 50 ml THF and then stirred for 2 hours under a nitrogen atmosphere at ambient temperature. Then 2.79 g (20 mmol) methyl 2-aminopropionate-hydrochloride and 50 ml THF are added and the mixture is stirred for a further 16 hours at ambient temperature. Then the reaction mixture is poured into water, extracted with ethyl acetate, the combined organic phases are washed with sat. sodium hydrogen carbonate solution, water, 0.5-molar hydrochloric acid, water and sat. sodium chloride solution, dried over magnesium sulphate and evaporated down completely i. vac.

1. stirringthe mixture is stirred for a further 16 hours at ambient temperature
2. extractionextracted with ethyl acetate
3. washthe combined organic phases are washed with sat. sodium hydrogen carbonate solution, water, 0.5-molar hydrochloric acid, water and sat. sodium chloride solution
4. dry with materialdried over magnesium sulphate
5. customevaporated down completely