Hydrochloric Acid → HCID 67517444, compound

Participants

Reaction Steps

A solution of tert-butyl 6-(methyl-(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)amino)-1,4-oxazepane-4-carboxylate (0.142 g, 0.283 mmole) 107.4 in MeOH (5 mL) was treated with 4 M HCl in 1,4-Dioxane (0.28 mL (1.13 mmol) and stirred at rt for 24 hr. An additional of 4 M HCl in 1,4-dioxane (0.4 mL) was added and the mixture stirred for an additional 24 hr and then heated at 50° C. for 2 hours. The mixture was cooled to rt and concentrated in vacuo to give a residue was dissolved in DCM (10 mL) and 5 mL MeOH and neutralized by addition of 0.43 g of polymer-supported carbonate resin (3.5 mmol/g) and stirring at room temperature for 2 hours. The resin was removed by filtered through celite, and the filtrate was concentrated to dryness to yield 125.6 mg of N-methyl-N-(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1,4-oxazepan-6-amine 107.5 as a yellowish solid glass that was used without further purification. LCMS (ESI) m/z: 402.20 [M+H]+.

Provenance & Evidence