HRID552372

反应详情

EQUATION

反应方程式

HRID 552372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-amino-6-nitro-benzoic acid (60 g, 329 mmol) and urea (257.3 g, 4285 mmol) in acetic acid (1.65 lit.) was heated to reflux for 24 h. The acetic acid was evaporated under reduced pressure and the residue obtained was diluted with water (2.5 lit). The solid product separated out was filtered and washed with water. The product was collected and dried in an air oven to give 44 g of the product as a yellow solid; 1H NMR (δ ppm, DMSO-d6, 300 MHz): 11.58 (br. s, 1H); 11.55 (br.s, 1H); 7.76 (t, J=8.4, 1H); 7.41 (d, J=7.8, 1H); 7.32 (d, J=8.4, 1H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 24 h
  3. customThe acetic acid was evaporated under reduced pressure
  4. customthe residue obtained
  5. customThe solid product separated out
  6. filtrationwas filtered
  7. washwashed with water
  8. customThe product was collected
  9. customdried in an air oven