HRID908394

反应详情

EQUATION

反应方程式

HRID 908394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Sodium triacetoxyhydroborate (25.9 mg) was added to 1-(4-bromo-3-methoxy-phenyl)piperazine (30 mg), N-ethyl-N-isopropyl-propan-2-amine (0.030 ml) and 37% aqueous formaldehyde (8.01 μl) dissolved in dichloromethane (1 ml). The resulting mixture was stirred at 25° C. for 2 hours. The reaction mixture was quenched with a saturated aqueous solution of sodium hydrogencarbonate (5 ml) and extracted with ethyl acetate (2×10 ml). The combined organic phases were dried over magnesium sulfate and concentrated to afford the crude 1-(4-bromo-3-methoxy-phenyl)-4-methyl-piperazine (25.00 mg). NMR Spectrum: (CDCl3) 2.38 (s, 3H), 2.60 (bs, 4H), 3.17-3.28 (m, 4H), 3.88 (s, 3H), 6.41 (dd, 1H), 6.47 (d, 1H), 7.36 (d, 1H); Mass spectrum: M+H+ 286

WORKUP

后处理

  1. customThe reaction mixture was quenched with a saturated aqueous solution of sodium hydrogencarbonate (5 ml)
  2. extractionextracted with ethyl acetate (2×10 ml)
  3. dry with materialThe combined organic phases were dried over magnesium sulfate
  4. concentrationconcentrated