HRID1272066
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4-Methoxymandelic acid (5.00 g, 27.44 mmol) was dissolved in 100 mL of THF. To this solution was added acetic anhydride (2.85 mL, 30.18 mmol), followed by Et3N (10 mL). The resulting mixture was stirred at room temperature overnight, concentrated, re-suspended in water, and extracted with EtOAc. The combined organic phase was dried over Na2SO4, and concentrated to give 5.95 g yellow syrup as the intermediate 79a. 1H NMR (300 MHz, CDCl3) δ 7.38 (d, 2H, J=8.67 Hz), 6.90 (d, 2H, J=8.67 Hz), 5.87 (s, 1H), 3.80 (s, 3H), 2.16 (s, 3H). LCMS (ESI−) [M−H]/z Calc'd 223, found 223.
WORKUP
后处理
- concentrationconcentrated
- extractionextracted with EtOAc
- dry with materialThe combined organic phase was dried over Na2SO4
- concentrationconcentrated