反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution consisting of 40 mL of acetic acid and 4 mL of concentrated sulfuric acid, was added 394 mg (0.753 mmol) of 10. The resulting mixture was refluxed for 4 hours. After allowing the mixture to cool to room temperature, the greyish colored precipitate was collected, washed with acetic acid, and then washed with water to afford pure 14 as a yellow solid: 260 mg (71%) yield; dec pt 290° C.; TLC (ethyl acetate/methanol [9:1]), Rf =0.56; IR (KBr pellet) 2967, 1687, 1630, 1599, 1497, 1463, 1427, 1239, 1206, 1066 cm-1 ; 1H NMR (dimethyl-d6 sulfoxide) δ7.32 (4H, t, J=7.4 Hz, aromatic, no assignments made), 7.08 (4H, d, J=7.8 Hz, aromatic, no assignments made), 6.98 (4H, t, J=7.4 Hz, aromatic, no assignments made), 5.02 (4H, s, methylenes), 3.81 (6H, s, methoxys); mass spectrum (EI mode), m/z 486 (P+). Anal. Calcd for C26H22N4O6 : C, 64.19; H, 4.56; N, 11.52. Found; C, 64.09; H, 4.52; N, 11.31.
WORKUP
后处理
- temperatureThe resulting mixture was refluxed for 4 hours
- customthe greyish colored precipitate was collected
- washwashed with acetic acid
- washwashed with water