HRID2065929

反应详情

EQUATION

反应方程式

HRID 2065929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
3 °C

PROCEDURE

实验过程

Ethyl 2-oxocyclohexane carboxylate (6, 484.9 g) and (S)-(−)-1-phenylethylamine (7, 362.5 g) were charged into an RB flask followed by heptanes (1.5 L) and Ytterbium (III) trifluoromethane sulfonate (8.8 g). The contents were heated to reflux for 3 hours and the liberated water was removed simultaneously and then cooled to 22° C. (±3° C.). The insoluble material was filtered and the filtrate was concentrate on a rotary evaporator under vacuum to afford 869.4 g of (S)-ethyl 2-(1-phenylethylamino)cyclohex-1-enecarboxylate (8) as an oil.

WORKUP

后处理

  1. temperatureThe contents were heated
  2. temperatureto reflux for 3 hours
  3. customthe liberated water was removed simultaneously
  4. filtrationThe insoluble material was filtered
  5. concentrationthe filtrate was concentrate on a rotary evaporator under vacuum