Hydrochloric Acid → HCID 86637006, compound

Participants

Reaction Steps

To a solution of tris(1,1-dimethylethyl)2-{2-chloro-6-[4-(dimethylamino)-2,2-dimethyl-1-pyrrolidinyl]-5-fluoro-4-pyrimidinyl}-1,1,2-hydrazinetricarboxylate (2.2004 g, 3.648 mmol) in MeOH (22 mL) was added 4 N HCl in dioxane (22 mL). The solution was stirred for 3 days and then concentrated in vacuo. The residue was azeotroped with MeOH (50 mL), and then partitioned between DCM (100 mL) and sat. aq. NaHCO3 (100 mL). The aqueous phase was extracted with fresh DCM (2×50 mL), and the combined organic phase was dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give 1-(2-chloro-5-fluoro-6-hydrazino-4-pyrimidinyl)-N,N,5,5-tetramethyl-3-pyrrolidinamine (1.0552 g, 96%) as an orange foam. LCMS: (M+H)+: 303.1.

Provenance & Evidence