HRID1502127
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
Ethyl 2-(6-methyl-5-(1H-tetrazol-1-yl)pyridin-2-yl)acetate (310 mg, 1.25 mmol) was dissolved in THF (6 mL) and water (3 mL). Lithium hydroxide monohydrate (68.31 mg, 1.628 mmol) was added. A small amount of ethanol was also added to ensure the reaction mixture was homogeneous. After 1 hr, the reaction was acidified with 2N HCl to pH ˜5-6 then extracted with a mixture of ethyl acetate/THF (2×). The combined organic layer was dried over Na2SO4, filtered and concentrated to yield title compound: 1H-NMR (600 MHz, CDCl3) δ ppm 8.975 (s, 1H), 7.738 (d, J=8.1 Hz, 1H), 7.396 (d, J=8.1 Hz, 1H), 3.907 (s, 2H), 2.009 (s, 3H): LC-MS: M+1=220
WORKUP
后处理
- extractionthen extracted with a mixture of ethyl acetate/THF (2×)
- dry with materialThe combined organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated