HRID1742424

反应详情

EQUATION

反应方程式

HRID 1742424 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 3-bromo-6,7-dihydro-5H-[1]pyrindine N-Oxide (250 mg, 1.17 mM) in 3 mL of CH2Cl2 at room temperature was added POCl3 (0.131 mL, 1.4 mM) and triethylamine (0.202 mL, 1.4 mM). The reaction was stirred at room temperature for 2 hours then was extracted from saturated NaHCO3 solution into ethyl acetate, washed with saturated NaCl, dried over MgSO4, filtered, and concentrated to dryness. The product was used crude in the next step. 1H NMR (CDCl3): d 8.60 (s, 1 H), 7.80 (s, 1 H), 5.40 (d, 1 H), 3.00 (m, 2 H), 2.20 (m, 2 H)

WORKUP

后处理

  1. extractionthen was extracted from saturated NaHCO3 solution into ethyl acetate
  2. washwashed with saturated NaCl
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated to dryness