Methanol → HCID 69652905, compound

Participants

Reaction Conditions

Reaction Steps

2-Chloro-6-[N-(trimethylsilylethoxycarbonyl)piperazinyl] purine (17.10 g, 44.66 mmol) and piperazine (23.08 g, 268 mmol) were suspended in EtOH (200 mL) in a bomb reactor. The bomb reactor was heated to 145° C. for 24 hours. The reaction progress was monitored by thin layer chromatography NH4OH:MeOH:EtOAc (5/5/90, v/v/v) which showed disappearance of starting material and formation of a new product spot after 24 hours. The EtOH was evaporated and water (700 mL) was added to the residue. The resulting precipitate was filtered and dried in a vacuum oven at 110° C. for 24 hours to give 18.5 g (96%) of the title compound. 1H NMR (CDCl3): δ 0.02 (s, 9H), 1.01 (t, 2H), 2.99 (bs, 4H), 3.61 (bs, 4H), 3.74 (bs, 6H), 4.23 (bm, 6H), 7.59 (s, 1H).

Provenance & Evidence