Phthalimide → HCID 178508598, compound

Participants

Reaction Steps

To a solution of 5 g (12.48 mmol) of trans-{3-[4-amino-5-(3-benzyloxy-phenyl)pyrrolo[2,3-d]pyrimidin-7-yl]-cyclobutyl}-methanol, which is prepared as described in Example 47(b) of WO 97/28161, in 100 ml of dry THF are added under argon 4.91 g (18.72 mmol) of triphenylphosphine and 2.75 g (18.7 mmol) of phthalimide; 3.36 g (3.02 ml; 18.7 mmol) of diethyl azodicarboxylate (96%) are added dropwise thereto. The reaction mixture is stirred at RT for 27 h. The reaction mixture is concentrated to dryness and the crude compound is purified by flash-chromatography (ethylacetate) to obtain trans-2-{3-[4-amino-5-(3-benzyloxy-phenyl)-pyrrolo[2,3-d]pyrimidin-7-yl]-cyclobutylmethyl}-isoindole-1,3-dione. Analytical HPLC: tR=12.12 min (Grad 1); ES-MS: m/eo=529.9.

Provenance & Evidence