HRID964566
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4-Methyldibenzofuran (30 g, 165 mmol) and sodium carbonate (17.5 g, 165 mmol) were mixed in hexane (300 ml) and bromine (26.4 g, 165 mmol) was added. The reaction was stirred at room temperature for 72 hours, then the solvent was removed in vacuo to give an oil which crystallised. Recrystallisation from IMS yielded several batches of off-white crystals (31.22 g, 72%) with m.p. 124°-125° C. (Found: C, 58.59; H, 3,28. C13H9BrO 0.31H2O requires: C, 58.58; H, 3.63%); δH [2H6 ]-DMSO 8.15 (1H, d), 7.9 (1H, d), 7.7 (1H, d), 7.4 (1H, t), 7.05 (2H, m), 2.6 (3H, s); m/z 260/262 (M+).
WORKUP
后处理
- customthe solvent was removed in vacuo
- customto give an oil which
- customcrystallised
- customRecrystallisation from IMS yielded several batches of off-white crystals (31.22 g, 72%) with m.p. 124°-125° C. (Found: C, 58.59; H, 3,28. C13H9BrO 0.31H2O requires: C, 58.58; H, 3.63%)