HRID646945

反应详情

EQUATION

反应方程式

HRID 646945 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of 1-[4-(4-methyl-3′-nitro-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-6′-yl)-piperazin-1-yl]-2-morpholin-4-yl-ethanone (as prepared in the previous step, 0.16 g, 0.37 mmol) in 2:1 EtOH:water (3 mL) was treated with NH4Cl (0.20 g, 3.7 mmol) and iron powder (0.10 g, 1.8 mmol). The reaction was heated to 100° C. for 50 min then cooled to room temperature. The mixture was neutralized with saturated aqueous NaHCO3 and extracted with CH2Cl2. The combined organic layers were dried over MgSO4 and concentrated in vacuo to afford the title compound (0.14 g, 100%), which was immediately used in the next reaction.

WORKUP

后处理

  1. temperaturethen cooled to room temperature
  2. extractionextracted with CH2Cl2
  3. dry with materialThe combined organic layers were dried over MgSO4
  4. concentrationconcentrated in vacuo