Toluene → HCID 59439477, compound

Participants

Reaction Conditions

Reaction Steps

202.2 g (2.020 mol) of 3-methylcrotonic acid and 2 L of methanesulfonic acid were put into a 10 L four-necked round bottom flask and stirred on a 50° C. water bath in stream of nitrogen. 500.0 g (1.836 mol) of 2-(2-hydroxy-6-methoxyphenyl)ethyl benzoate obtained in Example 4 was added to this solution. The reaction mixture was stirred at the same temperature for 1.8 hours and ice cooled. 2.5 L of toluene was added to the reaction mixture and subsequently 5 L of water was added dropwise for about 1 hour. The contents were transferred to a 20 L separatory funnel and allowed to be separated and the aqueous layer was discarded. The organic layer was washed three times with water (5 L×3) and concentrated in vacuo on a 40° C. bath and 846.1 g of the title compound was obtained.

Provenance & Evidence