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 ethyl 2-(3-benzoylureido)-4-(4-chlorobenzyl)-5-(3-chlorophenyl)furan-3-carboxylate (53.6 mg, 0.1 mmol) in EtOH (2 mL) was added sodium ethoxide (13.6 mg, 0.2 mmol). The reaction was heated at 100° C. (MW) for 20 min, cooled to RT and quenched with aq. NH4Cl (2 mL). The reaction was concentrated to a residue which was diluted with water (3 mL) and extracted with EA (3×8 mL). The combined organic layers were dried over Na2SO4 and concentrated to give 5-(4-chlorobenzyl)-6-(3-chloro phenyl)furo[2,3-d]pyrimidine-2,4(1H,3H)-dione (2.3 g, 83% yield) as a white solid. 1H NMR (DMSO-d6) δ: 9.70 (brd s, 1H), 7.38 (m, 3H), 7.33 (d, J=8.5 Hz, 2H), 7.30-7.21 (m, 3H), 4.24 (s, 2H). LCMS: MH+ 387 and TR=2.685 min. Used without further purification.
WORKUP
后处理
- temperatureThe reaction was heated at 100° C. (MW) for 20 min
- customquenched with aq. NH4Cl (2 mL)
- concentrationThe reaction was concentrated to a residue which
- additionwas diluted with water (3 mL)
- extractionextracted with EA (3×8 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- concentrationconcentrated