Formic Acid → 4-(Hydroxymethyl)-5-methyl-1,3-dioxol-2-one

Participants

Reaction Conditions

Reaction Steps

4-Chloromethyl-5-methyl-1,3-dioxol-2-one (25 g) was dissolved in dichloromethane (250 ml) at 20-25° C., sodium iodide (2.5 g) and formic acid (22 g) was added at 20-25° C. Resulting mixture was cooled to 10-15° C. and triethyl amine (46.8 g) was added at 10-15° C. in 20-25 minutes. Resulting mixture was stirred for 5.0-6.0 hrs at 40-45° C., cooled to 20-25° C. and added DM water (250 ml). Organic layer was separated and washed with brine solution, and distilled out. Residue was dissolved in methanol (300 ml), methanolic HCl was added drop wise and resulting mixture was stirred for 1 hrs at 60-65° C. Active charcoal (1 g) was added to the reaction mass and stirred for 20-25 minutes at 50-55° C. Reaction mass was filtered through hyflo bed and bed was washed by MeOH (12 ml). The filtrate was evaporated under vacuum at 40-45° C. Obtained product was diluted with ethyl acetate (75 ml) and evaporated under vacuum to remove methanol content. (Yield: 0.67 g; 76.5%)

Provenance & Evidence