Dichloromethane → HCID 20085079, compound

Participants

Reaction Steps

Alpha-methylstyrene (AMS) (2.0 L, 15.4 mole) is added slowly with stirring over 2 to 3 hours to a mixture of AlCl3 (0.7 g, 5.2 mmole) and dichloromethane (1.0 L, dried over 3 Å molecular sieves) in 4 L beaker, in a drybox at room temperature. After the addition of 1 L AMS, about 0.2 L dichloromethane is added to make up for the solvent evaporated due to the reaction exotherm. After the addition of all AMS, the reaction mixture is deactivated with 0.3 L methanol, washed three times with water, dried over calcium chloride, filtered and volatiles stripped first using a rotary evaporator and then high vacuum.

Provenance & Evidence