HRID1809149
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
To a 2 L pressure vessel was added 1-(3-nitrophenyl)-1H-tetrazole 10 (10.0 g, 52.3 mmol, 1.0 eq.) and methanol (500 mL). The resulting solution was purged with N2 for 5 min. 10% Pd/C (500 mg) was added to the solution and the vessel was placed on a Parr hydrogenator at 50 psi for 3 h. The Pd/C was removed by filtration and the filtrate was concentrated to yield a light gray solid (7.66 g, 91%). LC/MSD (HP Series 1100 MSD) MS (ES+) m/z 162.1 (M+H)+1 1H-NMR, Varian 400 MHz (DMSO-d) δ 9.96 (s, 1H), 7.23-7.19 (m, 1H), 7.01-7.00 (m, 1H), 6.93-6.91 (m, 1H), 6.70-6.67 (m, 1H), 5.64 (m, 2H) ppm.
WORKUP
后处理
- customThe resulting solution was purged with N2 for 5 min
- addition10% Pd/C (500 mg) was added to the solution
- customThe Pd/C was removed by filtration
- concentrationthe filtrate was concentrated