HRID516810

反应详情

EQUATION

反应方程式

HRID 516810 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-(2-hydroxy-3-phenoxypropyl)pyrrolidine-2,5-dione (3.5 g, 13.1 mmol) (as shown at 3 above) in HCl (12N, 20 mL) and ethanol (20 mL) was heated to reflux for 6 hours. After thin layer chromatography (TLC) showed the reaction was complete, the mixture was concentrated in vacuum to give a white residue, which was taken up in water (20 mL) and washed with ether (3*50 mL). The aqueous phase was concentrated to give crude product, which was crystallized from methanol to give 2.9 g of 1-amino-3-phenoxypropan-2-ol hydrochloride (as shown at 4).

WORKUP

后处理

  1. temperatureto reflux for 6 hours
  2. concentrationthe mixture was concentrated in vacuum
  3. customto give a white residue, which
  4. washwashed with ether (3*50 mL)
  5. concentrationThe aqueous phase was concentrated
  6. customto give crude product, which
  7. customwas crystallized from methanol