HRID660610
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 solution of 2,6-dimethoxy-N,N-dimethylbenzamide (100 mg, 0.48 mmol) in methylene chloride (2.5 mL) is added BBr3 (1.0M in methylene chloride, 1.4 mL) dropwise and the mixture is stirred at RT for 18 h. Water is added and the suspension is extracted with EtOAc. The organic layer is washed with water and brine, and dried over sodium sulfate. The solvent is removed under reduced pressure to give the title compound: 1H NMR (DMSO-d6) δ 9.35 (s, 2H), 6.93-6.89 (t, J=8.34 Hz, 1H), 6.29-6.27 (d, J=8.09 Hz, 2H), 2.89 (s, 3H), 2.86 (s, 3H).
WORKUP
后处理
- extractionthe suspension is extracted with EtOAc
- washThe organic layer is washed with water and brine
- dry with materialdried over sodium sulfate
- customThe solvent is removed under reduced pressure