Ethyl Acetate → HCID 68541607, compound

Participants

Reaction Conditions

Reaction Steps

Dissolve 2-chloro-3-methyl-5-nitropyridine (310 mg, 1.82 mmol, 1.0 equiv) and N—BOC-trans-2,5-dimethylpiperazine (397 mg, 2.0 mmol, 1.1 equiv) in 5 mL of anhydrous DMF, add potassium carbonate (251 mg, 1.82 mmol, 1.0 equiv) and stir the mixture for 20 hours at 80° C. Pour the solution in a 1:1 v/v mixture of EtOAc and iced water. Extract the aqueous phase with EtOAc (2×20 mL) and wash the combined organic layers with water (3×20 mL) and saturated aq. sodium chloride (30 mL). Dry the organic solution over sodium sulfate and concentrate under reduced pressure to obtained a crude rac-(trans)-2,5-dimethyl-4-(3-methyl-5-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester. MS(ES+): m/z=251.2 (M+H).

Provenance & Evidence