HRID1519531
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 the di-tert-butyl(3-bromo-4-cyanophenyl)malonate (2.2 g, 5.4 mmol) in dichloromethane (30 mL) was added triflouroacetic acid (10 mL) and the reaction mixture stirred for 12 h at room temperature. The solution was concentrated under reduced pressure and chased with toluene (2×) to give the crude product as a yellowish oil (1 g, 77%, and 85% purity as indicated by NMR). The residue was used in the next step without further purification. 1H NMR (500 MHz, DMSO-d6) δ 12.80 (br s, 1H), 7.87 (d, J=8 Hz, 1H), 7.80 (s, 1H), 7.48 (d, J=8 Hz, 1H), 3.73 (s, 2H). LC-MS (IE, m/z): 240 [M+1]+.
WORKUP
后处理
- concentrationThe solution was concentrated under reduced pressure and chased with toluene (2×)