HRID505356

反应详情

EQUATION

反应方程式

HRID 505356 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Imine 11b (10.74 g, 0.045 mol) was dissolved in methanol (100 mL) and NaBH4 (2×3 g) was added over 1 h while stirring the reaction mixture at room temperature. The reaction was quenched with methanol and the reaction mixture was concentrated and then diluted with diethyl ether (400 mL). The precipitate formed was removed by filtration. The filtrate was washed with water (2×200 mL), brine (200 mL), dried (Na2SO4) and concentrated to provide a yellow liquid (4.90 g, 46%). 1H NMR (300 MHz CDCl3) 6.79-6.69 (m, 3H), 5.86 (s, 2H), 4.41 (t, J=5.4 Hz, 1H), 3.64 (s, 2H), 3.30 (s, 6H), 2.65 (d, J=5.4 Hz, 2H).

WORKUP

后处理

  1. customThe reaction was quenched with methanol
  2. concentrationthe reaction mixture was concentrated
  3. additiondiluted with diethyl ether (400 mL)
  4. customThe precipitate formed
  5. customwas removed by filtration
  6. washThe filtrate was washed with water (2×200 mL), brine (200 mL)
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated