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
- 150 °C
PROCEDURE
实验过程
A suspension of 7-bromo-1H-isochromene-1,3(4H)-dione (1.09 g) and 3-amino-N-cyclopropyl-4-methylbenzamide (0.91 g) in a mixture of toluene (8 ml) and acetic acid (2.5 ml) was heated under microwave irradiation conditions (Personal Chemistry Emrys Optimizer with 300 W magnetron) at 150° C. for 60 minutes. This was process was repeated and the batches combined, diluted with ethyl acetate and washed with 1N HCl, saturated NaHCO3 solution, water, brine, dried (magnesium sulfate) to yield 3-(7-bromo-1,3-dioxo-3,4-dihydroisoquinolin-2(1H)-yl)-N-cyclopropyl-4-methylbenzamide as a brown solid (1.13 g); NMR Spectrum: (DMSOd6) 0.60 (m, 2H), 0.71 (m, 2H), 2.12 (s, 3H), 2.89 (m, 1H), 4.34 (d, 1H), 4.42 (d, 1H), 7.48 (d, 1H), 7.53 (d, 1H), 7.70 (s, 1H), 7.85 (d, 1H), 7.99 (d, 1H), 8.20 (s, 1H), 8.45 (d, 1H); Mass Spectrum: M+Na+ 435.
WORKUP
后处理
- washwashed with 1N HCl, saturated NaHCO3 solution, water, brine
- dry with materialdried (magnesium sulfate)