HRID497455
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
In a Paar flask 1-methyl-5-(3-nitrophenyl)-tetrazole (28.8 g, 140 mmol) was dissolved in ethyl acetate (430 mL) and methanol (1270 mL) and added to palladium on carbon (2.7 g, 10 wt %). The reaction mixture was hydrogenated for 1.5 hours with vigorous shaking. The reaction mixture was filtered, and concentrated in vacuo to give a white solid (24.0 g, 98%) was used with further purification. 1H NMR (300 MHz, CDCl3), δ: 7.21 (dd, J=8, J′=7, 1H), 6.99 (s, 1H), 6.90 (d, J=7, 1H), 6.76 (d, J=8, 1H), 5.44 (bs, 2H), 4.10 (s, 3H).
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- concentrationconcentrated in vacuo