Diethyl Ether → HCID 86616219, compound

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Reaction Steps

0.071 g of picolinoyl chloride and then 0.12 mL of DIPEA are added, at a temperature of 0° C., to a solution of 0.12 g of the compound prepared in step 2.2, in 1 mL of acetonitrile. The medium is stirred until it has returned to room temperature. After 1 hour at room temperature, the medium is hydrolysed and then diluted with EtOAc and washed with 10% Na2CO3 solution and then with saturated NaCl solution. After drying over MgSO4, the solution is concentrated. The crude product obtained is taken up in DCM. The hydrochloride is formed by addition of 2 M hydrochloric ethyl ether. The solid obtained is filtered off and rinsed with ethyl ether. The free base is obtained by treatment with 1 M sodium hydroxide and is then extracted into DCM and the organic phase is dried over MgSO4 and then evaporated. The free base is taken up in DCM. The hydrochloride is obtained by addition of 2 M hydrochloric ethyl ether. The solid obtained is filtered off, rinsed with ethyl ether and then dried to give 91 mg of a white solid.

Provenance & Evidence