Dimethylformamide → HCID 11402394, compound

Participants

Reaction Conditions

Reaction Steps

16.5 g (0.05 mol) of the obtained 5-bromo-2,5-dimethyl-2-(1-adamantyl)-1,3-dioxolan-4-one was placed in a 100 ml egg-plant type flask, and 73.1 g (1.0 mol) of N,N-dimethylformamide was added thereto, followed by intensively stirring at 40° C. for 2 hours. After completion of the stirring, the mixture was transferred into a 500 ml separatory funnel, and 200 g of isopropyl ether was added thereto, followed by fully shaking. Thereafter, the obtained mixture was left at rest, so as to separate the mixture into two layers. And then, the N,N-dimethylformamide phase that was a lower layer was removed. The isopropyl ether phase that was a upper layer washed with water to remove N,N-dimethylformamide dissolved therein. Thereafter, isopropyl ether was removed, so as to obtain white crystals. The obtained white crystals were recrystallized from hexane, so as to obtain 10.9 g of 5-methylene-2-(1-adamantyl)-2-methyl-1,3-dioxolan-4-one at a purity of 99.8% (Formula (19), yield: 88%).

Provenance & Evidence