HRID1753758

反应详情

EQUATION

反应方程式

HRID 1753758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of NaOEt in dry EtOH (45 mL, 114.90 mmol) under inert atmosphere was added 4-chloromethyl-1-methyl-2-nitro-benzene (7.0 g, 38.30 mmol). The reaction mixture was stirred at room temperature for 16 hours. Water was added and ethanol was removed under reduced pressure. The crude product was extracted with DCM (2 times) and the organic layer was washed with water, then with a saturated solution of NaCl, dried over MgSO4 and concentrated to give I-g as brown oil in 96% yield. 1H NMR (300 MHz, CDCl3) δ 7.95 (s, 1H), 7.48 (d, J=7.8 Hz, 1H), 7.31 (d, J=7.9 Hz, 1H), 4.52 (s, 2H), 3.56 (q, J=7.0 Hz, 2H), 2.57 (d, J=10.1 Hz, 3H), 1.26 (t, J=7.0 Hz, 3H).

WORKUP

后处理

  1. customethanol was removed under reduced pressure
  2. extractionThe crude product was extracted with DCM (2 times)
  3. washthe organic layer was washed with water
  4. dry with materialwith a saturated solution of NaCl, dried over MgSO4
  5. concentrationconcentrated
  6. customto give I-g as brown oil in 96% yield