反应详情

First N-methyl-morpholine (4 eq.) and then HATU (2.0 eq.) was added to a solution of N-Boc-sarcosine (30.12 mmol, 1.0 eq.) in DMF (3 ml/mmol) at 0° C. The reaction mixture was stirred at room temperature for 15 min and then cooled again to 0° C. in order to add a solution of methyl 2,3-diaminobenzoate (30.12 mmol, 1.0 eq.) in DMF (1 ml/mmol). The reaction mixture was then stirred at room temperature for 16 h. For working up, the reaction mixture was diluted with water and extracted with ethyl acetate and the organic phase was washed with sat. NH4Cl solution, sat. NaHCO3 solution and sat. NaCl solution. The organic phase was dried over Na2SO4 and concentrated in vacuo in order to obtain the crude product. This was purified by a column chromatography (silica gel) to obtain the desired product. Yield: 60%

1. temperaturecooled again to 0° C. in order
2. stirringThe reaction mixture was then stirred at room temperature for 16 h
3. extractionextracted with ethyl acetate
4. washthe organic phase was washed with sat. NH4Cl solution, sat. NaHCO3 solution and sat. NaCl solution
5. dry with materialThe organic phase was dried over Na2SO4
6. concentrationconcentrated in vacuo in order
7. customto obtain the crude product
8. customThis was purified by a column chromatography (silica gel)