反应详情

A solution of 5,5-dimethyl-cyclohexane-1,3-dione (80.0 g, 0.57 mol) in anhydrous methanol (600 mL) was treated with a 1 M solution of titanium chloride (TiCl4) in dichloromethane (17.2 mL). After stirring 1 hour at room temperature, the mixture was slowly poured into cold 5% NaHCO3 solution and extracted with diethyl ether (450 mL×6). The organic layers were collected, washed with brine, dried on Na2SO4 and evaporated to dryness affording the title compound (81.5 g, 92% yield) as a pale yellow oil.

1. extractionextracted with diethyl ether (450 mL×6)
2. customThe organic layers were collected
3. washwashed with brine
4. customdried on Na2SO4
5. customevaporated to dryness