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0 °C

To a stirred solution of 4-(5-cyano-[1,3,4]thiadiazol-2-ylamino)-piperidine-1-carboxylic acid tert-butyl ester (D5) (0.973 g, 3.12 mmol) in dichloromethane (55 ml), at 0° C., was added trifluoroacetic acid (3 ml). The reaction mixture was stirred at 0° C. for 1 h. and at room temperature for 18 h. more. After this period, the reaction mixture was extracted with a saturated solution of sodium carbonate. The aqueous layer was extracted with ethyl acetate (2×25 ml). The organic layer was separated, dried (Na2SO4) and the solvent evaporated in vacuo to yield D6 (0.60 g, 92%) as a solid. C8H11N3S requires 209. Found 210 (MH+).

1. waitAfter this period
2. extractionthe reaction mixture was extracted with a saturated solution of sodium carbonate
3. extractionThe aqueous layer was extracted with ethyl acetate (2×25 ml)
4. customThe organic layer was separated
5. dry with materialdried (Na2SO4)
6. customthe solvent evaporated in vacuo