Sodium Carbonate → HCID 71182917, compound

Participants

Reaction Steps

2-(4-amino-2-fluorophenyl)-hexahydro-1H-spiro[cyclopenta[c]pyrrol-5,2′-[1,3]dioxolane] (74.7 mmol) prepared in the step 5 was dissolved in 300 ml of acetone, and 150 ml of a 10 wt % sodium carbonate aqueous solution was added. And then, the temperature was lowered to 0° C., 13.86 ml (97.1 mmol) of benzyl chloroformate was slowly added dropwise over 30 minutes, and the mixture was stirred for 12 hours while raising the temperature to room temperature. After the reaction was completed, the solvent was removed under reduced pressure, 300 ml of ethyl acetate was added, the mixture was washed with water and sodium chloride, and then, the organic layer was dried over magnesium sulfate and filtered and concentrated under reduced pressure. The concentrate was separated by column chromatography to obtain 24.1 g (78%) of the title compound, of which NMR data is as follows.

Provenance & Evidence