HRID2046553
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- additionAfter the addition
- temperaturethe brown mixture was heated
- temperatureto reflux for 3 h
- concentrationwas concentrated to dryness
- customto remove acetic acid and water
- customThe remaining brown oil was purified by chromatography (silica gel; CH2Cl2/EtOAc 100:0-0:100)