HRID1061216

反应详情

EQUATION

反应方程式

HRID 1061216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(1,4-dioxa-8-aza-spiro[4.5]dec-8-yl)-benzaldehyde(Taylor, E. C., Skotnicki, J. S. Synthesis, 1981, 606) (4.96 g, 20 mol), rhodanine (2.66 g, 20 mmol), and β-alanine (2.0 g, 22.5 mmol) in 50 mL of acetic acid (AcOH) was refluxed for 2 hours. The solid which was formed on cooling the solution was collected to give the title compound as a red solid (4.8 g, 66%); 1H NMR (300 MHz, CDCl3) δ 1.81 (t, J=5.5 Hz, 4H), 3.55 (t, J=5.5 Hz, 4H), 4.00 (s, 4H), 6.92 (d, J=8.9 Hz, 2H), 7.58 (d, J=8.9 Hz, 2H), 7.38 (s, 1H); MS (ES) m/z: 362.8 (MH+); HRMS Calcd. for C17H19N2O3S2 (MH+): 363.0837. Found: 363.0852. Anal. Calcd. for C17H18N2O3S2: C, 56.33; H, 5.01; N, 7.73. Found: C, 56.28; H, 4.89; N, 7.73.

WORKUP

后处理

  1. temperaturewas refluxed for 2 hours
  2. customThe solid which was formed
  3. temperatureon cooling the solution
  4. customwas collected