HRID1029500

反应详情

EQUATION

反应方程式

HRID 1029500 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 4-diisopropylaminobutyrate may be obtained in the following manner: diisopropylamine (40.4 g) is added dropwise to a solution of ethyl 4-bromobutyrate (39 g) in ethanol (80 cc). The solution obtained is heated to reflux for 6 hours. After the insoluble material formed has been filtered off, the filtrate is concentrated to dryness under reduced pressure (2.7 kPa). The residue is taken up with distilled water (15 cc) and 4 N aqueous hydrochloric acid solution (100 cc). The aqueous phase is washed with ethyl ether (3×75 cc) and then alkalinized with 10 N aqueous sodium hydroxide solution. The oil formed is extracted with ethyl ether (3×75 cc). The organic phase obtained is concentrated to dryness under reduced pressure (2.7 kPa). Ethyl 4-diisopropylaminobutyrate (9.2 g) is thereby obtained in the form of an oil, which is employed in the crude state in the subsequent syntheses.

WORKUP

后处理

  1. customThe solution obtained
  2. temperatureis heated
  3. temperatureto reflux for 6 hours
  4. customAfter the insoluble material formed
  5. filtrationhas been filtered off
  6. concentrationthe filtrate is concentrated to dryness under reduced pressure (2.7 kPa)
  7. washThe aqueous phase is washed with ethyl ether (3×75 cc)
  8. customThe oil formed
  9. extractionis extracted with ethyl ether (3×75 cc)
  10. customThe organic phase obtained
  11. concentrationis concentrated to dryness under reduced pressure (2.7 kPa)