HRID414699

反应详情

EQUATION

反应方程式

HRID 414699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride (NaBH4) (0.2 g, 5.8 mmol) was added to a slurry of the cinnamic ester (2) (3.4 g, 10.5 mmol) in 100 mL of absolute ethanol and the reaction allowed to stir at room temperature for 1.5 hours. Acetic acid (0.5 mL) was added and the mixture concentrated. The residue was dissolved in 250 mL of CHCl3 and was washed with 100 mL of saturated sodium bicarbonate (NaHCO3) solution, and H2O (100 mL). The organic phase was separated, dried (Na2SO4) and concentrated to produce 3.1 g of an orange solid. An analytical sample was obtained by crystallization from methanol(MeOH)-water, m.p. 75°-77° C.

WORKUP

后处理

  1. concentrationthe mixture concentrated
  2. dissolutionThe residue was dissolved in 250 mL of CHCl3
  3. washwas washed with 100 mL of saturated sodium bicarbonate (NaHCO3) solution, and H2O (100 mL)
  4. customThe organic phase was separated
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated