HRID1684105

反应详情

EQUATION

反应方程式

HRID 1684105 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe resulting mixture was refluxed for 4 hours
  2. customthe greyish colored precipitate was collected
  3. washwashed with acetic acid
  4. washwashed with water