HCID 178427769, compound → HCID 178421987, compound

Participants

Reaction Steps

0.335 g (0.589 mmol) trans-toluene-4-sulfonic acid 3-[4-amino-5-(3-benzyloxy-phenyl)-6-methyl-pyrrolo[2,3-d]pyrimidin-7-yl]-cyclobutylmethyl ester of Example 106 in 3.6 ml pyrrolidine are stirred at RT for 3.5 h (Thin Layer Chromatography and HPLC control). The excess reagent is evaporated on a rotavap and the residue purified by chromatography (solvent: ethyl acetate-MeOH-aqu. NH3 (33%) 95:5:1). The compound is crystallized from diethylether. Analytical HPLC: tR=9.09 min (Grad 1); mp: 136-140° C.; ES-MS: m/eo=468.3; NMR (DMSO-d6; not all signals reported): 8.10/s (1H), 7.25-7.5/several m's (6H), 7.02/“d” (1H); 6.94/s (1H); 6.89/“d” (1H); 5.5-6.0/b (NH2); 5.13/s (2H); 5.06/m (1H); 2.22/s (3H).

Provenance & Evidence