HRID2211881

反应详情

EQUATION

反应方程式

HRID 2211881 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A round bottomed flask was charged with 6.51 g (0.028 mol) of 3-methyl-2nitrobenzyl bromide, 120 mL 1:1 EtOH:H2O, and 5.5 g KCN (0.084 mol). The reaction solution was heated to 60° C. for 2 h. The reaction was cooled and the volatiles removed in vacuo. The resulting solid was dissolved in 150 mL water and extracted with 300 mL ethyl acetate. The organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated. This gave 4.63 g (92% yield) of the desired material as a slightly yellow solid. 1H NMR (400 MHz, CDCl3) δ 7.45–7.41 (m, 2H), 7.33–7.31 (m,1H), 3.77 (s, 2H), 2.36 (s, 3H).

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. customthe volatiles removed in vacuo
  3. dissolutionThe resulting solid was dissolved in 150 mL water
  4. extractionextracted with 300 mL ethyl acetate
  5. washThe organic extracts were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated