HRID1469724

反应详情

EQUATION

反应方程式

HRID 1469724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 8-nitroquinazolin-4(3H)-one (1.0 g, 5.23 mmol) and PCl5 (1.3 g, 6.24 mmol) in POCl3 (5 mL) was heated at reflux for 4 h. Then the reaction mixture was concentrated and the concentrate was diluted with Et2O. The precipitated solid was filtered and dried to afford 1.0 g of the title product. 1H NMR (300 MHz, DMSO d6): δ 9.25 (s, 1H), 8.71 (d, J=7.8 Hz, 1H), 8.59 (d, J=7.8 Hz, 1H), 8.07-8.02 (t, J=7.8 Hz, 1H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 4 h
  3. concentrationThen the reaction mixture was concentrated
  4. additionthe concentrate was diluted with Et2O
  5. filtrationThe precipitated solid was filtered
  6. customdried