HRID495690

反应详情

EQUATION

反应方程式

HRID 495690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 100 ml 2-necked flask equipped with a reflux condenser, a thermometer, a magnetic stirrer and an inert gas supply, 20 ml tetrahydrofuran were added to 2.3 ml (R)-phenyloxirane (20 mmol) and 1.03 g magnesium bromide ethyl etherate (4 mmol) were dissolved therein. The yellowish solution was mixed with 4.9 ml diallylamine and refluxed for 2 h. The orange-brown solution was cooled to room temperature, stirred for 15 min with 20 ml 5M ammonium chloride solution and the aqueous phase was separated. The organic phase was dried with 8.5 g sodium sulfate, filtered and washed with 10 ml tetrahydrofuran. The solvent was concentrated and the orange-brown oil was dried during 1 h to yield 4.2 g (97%) of (S)-2-(N,N-diallylamino)-2-phenylethanol and (R)-2-(N,N-diallylamino)-1-phenylethanol.

WORKUP

后处理

  1. customIn a 100 ml 2-necked flask equipped with a reflux condenser
  2. dissolutionwere dissolved
  3. temperaturerefluxed for 2 h
  4. customthe aqueous phase was separated
  5. dry with materialThe organic phase was dried with 8.5 g sodium sulfate
  6. filtrationfiltered
  7. washwashed with 10 ml tetrahydrofuran
  8. concentrationThe solvent was concentrated
  9. customthe orange-brown oil was dried during 1 h