preparation | (R)-3-(methylamino) pyrrolidine carboxylic acid dissolved in of an aqueous solution of sodium hydroxide, add 200ml of tetrahydrofuran and 250g of di-tert-butyl dicarbonate sequentially, control the pH value to 8-9, react for 12h, extract twice with ethyl acetate, 500ml each time; Then acidify the aqueous phase with HCI to pH value of 1-2, the product was extracted three times with 200ml of ethyl acetate each time; The ester layers were combined and washed twice with ml of saturated brine each time. Dry over anhydrous sodium sulfate for 12h, filter, concentrate the crystals, and dry at 40-50 °c to give tert-butyl (R)-3-(methylamino) pyrrolidine carboxylate. |