HRID1464630

反应详情

EQUATION

反应方程式

HRID 1464630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
133 °C

PROCEDURE

实验过程

A seated tube containing 2-chloro-5,6,7,8-tetrahydroquinoxaline (1.51 g, 0.009 mol), concentrated NH4OH (10 mL), isopropyl alcohol (30 mL), and copper powder (300 mg) was heated in an oil bath at 133° C. for 20 hours. The cooled mixture was filtered through celite and washed through the filter agent with H2O and hexanes. The layers were separated and the aqueous portion was washed (2×) with hexanes in order to remove unreacted starting material and then extracted with EtOAc (4×). The combined EtOAc extracts were dried over sodium sulfate and concentrated under reduced pressure to yield 2-amino-5,6,7,8-tetrahydroquinoxaline as a yellow-green solid.

WORKUP

后处理

  1. filtrationThe cooled mixture was filtered through celite
  2. washwashed through the filter agent with H2O and hexanes
  3. customThe layers were separated
  4. washthe aqueous portion was washed (2×) with hexanes in order
  5. customto remove unreacted
  6. extractionextracted with EtOAc (4×)
  7. dry with materialThe combined EtOAc extracts were dried over sodium sulfate
  8. concentrationconcentrated under reduced pressure