反应详情

温度

50 °C

3.10 g (30.96 mmol) N-hydroxy-cyclopropanecarboxamidine are placed in 10 ml dimethylformamide and molecular sieve. 1.32 g (34.06 mmol) sodium hydride (60% in mineral oil) are added. The mixture is stirred for 0.1 hours at 50° C., then 7.40 g (34.06 mmol) ethyl 3-tert-butoxycarbonylamino-propionate in 20 ml dimethylformamide are added. The reaction mixture is stirred for 3 hours at 50° C. After cooling 15 ml of water are added, the mixture is suction filtered through Celite. The 2 phases of the filtrate are separated, the aqueous phase is extracted with ethyl acetate, the combined organic phase is evaporated down. The residue is purified by chromatography.

1. stirringThe reaction mixture is stirred for 3 hours at 50° C
2. additionare added
3. filtrationfiltered through Celite
4. customThe 2 phases of the filtrate are separated
5. extractionthe aqueous phase is extracted with ethyl acetate
6. customthe combined organic phase is evaporated down
7. customThe residue is purified by chromatography