HRID2227451

反应详情

EQUATION

反应方程式

HRID 2227451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of propiophenone (30 g), KCN (34.5 g) and NH4Cl (30 g) in 180 mL of conc. NH4OH and 120 mL of EtOH is stirred at ambient temperature for 4 days. The reaction mixture is concentrated under vacuum and ether was added to the solid residue. The ether suspension is filtered and solid is washed with ether. Excess 1M of HCl in ether is added to the filtrate to precipitate HCl salt. The white solid is collected by filtration, washed with hexane and ether, and dried to give 29 g of the title compound as HCl salts. The white solid is basified with excess aqueous NaHCO3 and extracted with CH2Cl2. The extract is washed with brine, dried and concentrated to give 19 g of the titled compound as clear oil.

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated under vacuum and ether
  2. additionwas added to the solid residue
  3. filtrationThe ether suspension is filtered
  4. washsolid is washed with ether
  5. additionExcess 1M of HCl in ether is added to the filtrate
  6. customto precipitate HCl salt
  7. filtrationThe white solid is collected by filtration
  8. washwashed with hexane and ether
  9. customdried