HRID2046553

反应详情

EQUATION

反应方程式

HRID 2046553 的结构方程式

PROCEDURE

实验过程

To a mixture of 2-(5-bromo-indan-1-ylidene)-[1,3]dithiane (2.02 g, 6.45 mmol) in acetic acid (34 ml) was added 37% HCl (11 ml). After the addition, the brown mixture was heated to reflux for 3 h; then, the reaction mixture was allowed to cool to room temperature and was concentrated to dryness, using toluene as co-evaporating solvent to remove acetic acid and water. This process was repeated four times. The remaining brown oil was purified by chromatography (silica gel; CH2Cl2/EtOAc 100:0-0:100) to obtain the title compound as light brown solid (1.335 g, 86%). MS: 238.6 [M−H]−.

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturethe brown mixture was heated
  3. temperatureto reflux for 3 h
  4. concentrationwas concentrated to dryness
  5. customto remove acetic acid and water
  6. customThe remaining brown oil was purified by chromatography (silica gel; CH2Cl2/EtOAc 100:0-0:100)