反应详情

温度

50 °C

A mixture of 4-cyano-2-fluorobenzyl bromide (250 g, 1.17 mol), sarcosine tert-butyl ester hydrochloride (212.2 g, 1.17 mol) and potassium carbonate (484 g, 3.50 mol) in acetone (2 L) was stirred 24 hours at 50° C. and 18 hours at RT. The reaction mixture was filtered and the filtrate was concentrated under vacuum. The residue was taken up with water (1 L) and extracted with ethyl acetate (2×1 L). The combined organic layers were washed with water (1 L), dried (MgSO4) and concentrated under vacuum to give the title compound as a yellow-brown oil (325 g, quantitative). 1H NMR (DMSO-d6, 300 MHz) δ 7.82 (dd, J=9.9, 1.4 Hz, 1H), 7.70 (dd, J=7.9, 1.5 Hz, 1H), 7.64 (m, 1H), 3.78 (s, 2H), 3.23 (s, 2H), 2.27 (s, 3H), 1.42 (s, 9H). LC/MS (Method B): 279.2 (M+H)+.

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate was concentrated under vacuum
3. extractionextracted with ethyl acetate (2×1 L)
4. washThe combined organic layers were washed with water (1 L)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated under vacuum