HRID2255481
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
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).
WORKUP
后处理
- waitleft
- filtrationThe suspension was filtered
- washwashing with ethyl acetate
- customto give a solid which
- customwas recrystallized from methanol/water/isopropanol (final volume 50 mL)