HRID719872

反应详情

EQUATION

反应方程式

HRID 719872 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of N-(5-nitro-pyrazin-2-yl)-methanesulfonamide (583.9 mg, 2.67 mmol) in methanol (26.8 mL) was treated with a solution of ammonium chloride (300.6 mg, 5.62 mmol) in water (2 mL). This solution was stirred at 25° C. for 5 min. At this time, the reaction was treated with zinc dust (1.71 g, 26.2 mmol). The resulting mixture was heated under reflux for 2 h. At this time, the reaction was cooled to 25° C. and was filtered through a pad of silica gel (9/1 methylene chloride/methanol wash). The filtrate was concentrated in vacuo to afford N-(5-amino-pyrazin-2-yl)-methanesulfonamide (548.8 mg, 100%) as a dark-brown gum: EI-HRMS m/e calcd for C5H8N4O2S (M+H)+ 189.0441, found 189.0442.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 2 h
  3. temperatureAt this time, the reaction was cooled to 25° C.
  4. filtrationwas filtered through a pad of silica gel (9/1 methylene chloride/methanol wash)
  5. concentrationThe filtrate was concentrated in vacuo