HRID500659
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
- 200 °C
PROCEDURE
实验过程
[2-(ethoxycarbonyl)-1-benzothien-6-yl]malonic acid (0.60 g, 1.95 mmol) was suspended in H2O (4 mL) before heating at 200° C. in a microwave reactor for 60 seconds. The suspension was diluted with H2O (50 mL) and the products extracted into EtOAc (3×75 mL). The combined organic extracts were washed with brine, dried over MgSO4 and concentrated in vacuo to give 0.51 g of product (white solid, 99%). 1H NMR (DMSO-d6) δ 12.42 (br s, 1H), 8.15 (s, 1H), 7.94 (d, J=8.4 Hz, 1H), 7.91 (s, 1H), 7.35 (dd, J=8.4, 1.8 Hz, 1H), 4.32 (q, J=7.2 Hz, 2H), 3.71 (s, 2H), 1.32 (t, J=7.2 Hz, 3H).
WORKUP
后处理
- extractionthe products extracted into EtOAc (3×75 mL)
- washThe combined organic extracts were washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo