HRID2041010

反应详情

EQUATION

反应方程式

HRID 2041010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-amino-4-hydroxybenzoate (5.09 g, 30.4 mmol) and potassium O-ethyl carbonodithioate (6.35 g, 39.6 mmol) were combined in pyridine (50 mL) and heated to reflux for two hours. The reaction mixture was cooled to ambient temperature. The mixture was filtered, washed with a 1 N aqueous hydrochloric acid solution, and dried on a vacuum filter overnight to afford the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 3.88 (s, 3 H) 7.63 (d, J=8.48 Hz, 1 H) 7.69 (d, J=1.70 Hz, 1 H) 7.89 (dd, J=8.82, 1.70 Hz, 1 H); MS (ESI−) m/z 207.87 (M−H)−.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for two hours
  3. filtrationThe mixture was filtered
  4. washwashed with a 1 N aqueous hydrochloric acid solution
  5. customdried on a vacuum
  6. filtrationfilter overnight