HRID1742416
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
CONDITIONS
反应条件
- 温度
- 23 °C
PROCEDURE
实验过程
A mixture of 2-[1-(2-ethyl-5,7-dimethyl-imidazo[4,5-b]pyridin-3-yl)-indan-5-yl]-benzonitrile (100 mg, 0.26 mmol) and trimethyltin azide (110 mg, 0.51 mmol) in xylene (3.0 mL) was heated under reflux for 48 hours. The reaction mixture was cooled to 23° C. and the solvent was removed in vacuo. The crude residue was chromatographed on SiO2 -gel using 10% MeOH/CH2Cl2 to afford 45 mg of the tetrazole, mp-181 ° C. 1H NMR (250 MHz, d6 -DMSO): d 7.64 (m, 1 H), 7.53 (m, 1 H), 7.15 (s, 1 H), 6.91 (s, 1 H), 6.80 (d, 1 H), 6.70 (d, 1 H), 6.48 (m, 1 H), 3.04 (m,2 H), 2.68 (2H, m) 2.49 (s, 3 H), 2.42 (s, 3 H), 1.25 (t, 3 H); MS (M+): 435
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 48 hours
- customthe solvent was removed in vacuo
- customThe crude residue was chromatographed on SiO2