HRID618751
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
5.89 g of triethylamine, 8.14 g of triphenylchloromethane and 0.10 g of 4-N,N-dimethylaminopyridine are added in succession to a suspension of 10.37 g of 3-bromo-2-[2'-(1H-tetrazol-5-yl)-phenyl]-5-methylbenzofuran in 300 ml of CH2Cl2 and the batch is stirred for 3 hours at room temperature. The reaction solution is washed with 150 ml of water and 150 ml of brine, concentrated in vacuo to a volume of 50 ml and chromatographed on silica gel 60 (40-63 μm) using CH2Cl2 as eluant. The product, of Rf =0.82 (CH2Cl2 /CH3OH (95:5)), yields crystalline 3-bromo-2-[2-(1-trityltetrazol-5-yl)-phenyl]-5-methylbenzofuran, m.p. 199-200°, from ether.
WORKUP
后处理
- washThe reaction solution is washed with 150 ml of water and 150 ml of brine
- concentrationconcentrated in vacuo to a volume of 50 ml
- customchromatographed on silica gel 60 (40-63 μm)