HRID1731144

反应详情

EQUATION

反应方程式

HRID 1731144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 1-dimethylamino-3-butanone (1.0 g) dissolved in toluene (10 ml), p-toluenesulfonic acid (1.3 g) is added. The suspension is stirred for 10 min. Indene-3-ethanol (1.0 g) in toluene (5 ml) is added to the suspension and the resulting solution stirred for 2 hr. Boron trifluoride etherate (0.25 ml) is added together with ca. 0.5 g of hydrated alkali-aluminum silicate. The mixture is heated at 80° C for 30 min. The mixture is cooled and diluted with water. The organic layer is separated and the aqueous layer extracted with toluene. The organic layers are washed with water. The combined aqueous phase is rendered alkaline with conc.NH4OH and extracted with toluene. The latter extract is treated with charcoal and then concentrated to afford the title compound, identical to the compound of the same name described in Example 284.

WORKUP

后处理

  1. stirringthe resulting solution stirred for 2 hr
  2. temperatureThe mixture is cooled
  3. customThe organic layer is separated
  4. extractionthe aqueous layer extracted with toluene
  5. washThe organic layers are washed with water
  6. extractionNH4OH and extracted with toluene
  7. extractionThe latter extract
  8. additionis treated with charcoal
  9. concentrationconcentrated