Diethylamine → HCID 178464108, compound

Participants

Reaction Steps

To a solution of 0.2 g (0.5 mmol) of trans-7-(3-aminomethyl-cyclobutyl)-5-(3-benzyloxy-phenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine in 5 ml of dichloromethane are added 55.4 μl (0.5 mmol) of 2-bromoethyl chloroformate (Fluka, Buchs, Switzerland) and 70 μl (0.5 mmol) of triethylamine. After stirring for 2 h at RT, the solution is concentrated to dryness. The crude compound is dissolved in 5 ml of acetonitrile and 260 μl (2.5 mmol) of diethylamine (Fluka, Buchs, Switzerland) are added thereto. The reaction mixture is refluxed for 16 h and, after concentration, the crude compound is purified by medium-pressure liquid chromatography to provide trans-{3-[4-amino-5-(3-benzyloxy-phenyl)pyrrolo[2,3-d]pyrimidin-7-yl]-cyclobutylmethyl}-carbamic acid 2-diethylamino-ethyl ester. Analytical HPLC: tR=6.27 min (Grad 2); ES-MS: m/eo=543.3.

Provenance & Evidence