Piperidine → HCID 67288919, compound

Participants

Reaction Conditions

Reaction Steps

162 g (1.47 mol, 1.05 eq) of N-methylmorphorine was added to the mixed solution of 278 g (1.4 mol, 1.0 eq) of 2-fluoro-3-(methoxycarbonyl)benzoic acid obtained from the Step 2 and 2.7 l of dichloromethane, and then stirred for 30 minutes at 0° C. 191 ml (1.47 mol, 1.05 eq) of isobutyl chloromate was slowly added, and then stirred for 1 hour at 0° C. 139 ml (1.4 mol, 1.0 eq) of piperidine was slowly added, and then stirred for 1 hour at a room temperature. After completing the reaction, the reaction solution was washed with 560 ml of a saturated sodium bicarbonate aqueous solution, 560 ml of a saturated ammonium chloride aqueous solution, and 1 l of distilled water in order. A obtained organic layer was dehydrated with magnesium sulfate anhydrous, filtered, and then concentrated under reduced pressure to obtain 371 g of methyl 2-fluoro-3-(piperidine-1-carbonyl)benzoate in a red-yellow oil phase

Provenance & Evidence