反应详情

An ethanolic (86 mL) solution of (8,9-dioxo-2,6-diazabicyclo[5.2.0]non-1-(7)-en-2-yl)acetic acid 1,1-dimethylethyl ester (2.29 g, 8.60 mmol) was treated at room temperature with 2.5N sodium hydroxide solution (3.5 mL, 8.7 mmol) and left stirring overnight. The suspension was filtered, washing with ethyl acetate to give a solid which was recrystallized from methanol/water/isopropanol (final volume 50 mL) to afford (8,9-dioxo-2,6-diazabicyclo[5.2.0]non-1(7)-en-2-yl)acetic acid sodium salt hydrate (1.43 g, 66%, mp 280°-300° C. dec); MS (-FAB): 231 (M-H, 37), 209 (M-Na, 100); 1H NMR (DMSO 1 drop of DCl, 400 MHz): δ 4.40 (s, 2H), 3.36-3.25 (m, 4H), 1.89 (m, 2H).

1. waitleft
2. filtrationThe suspension was filtered
3. washwashing with ethyl acetate
4. customto give a solid which
5. customwas recrystallized from methanol/water/isopropanol (final volume 50 mL)