Dimethylformamide dimethyl acetal → HCID 68117268, compound

Participants

Reaction Steps

5.95 g of N,N-dimethyl formamide dimethyl acetal in 25 ml of chloroform was added dropwise at room temperature to a mixture of 8.0 g of 2 b in 50 ml of chloroform and the mixture was stirred for one hour at room temperature, then was heated to reflux and stirred for 12.5 hours. The solvent then was evaporated under reduced pressure to give a mushy solid, which was passed through fluorosil, using methylene chloride, then methanol, as eluents. The resulting material then was passed through fluorosil using a 99:1 mixture of methylene chloride and methanol as eluent to give 21 as a yellow solid, m.p.: 171°-172°.

Provenance & Evidence