HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl piperazine-1-carboxylate → HCID 16035853, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | HCID 57722777 | HCID 57722777 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 16035853 | HCID 16035853 | — |
Reaction Steps
3-chloro-7-oxiran-2-yl-5H-benzo[4,5]cyclohepta[1,2-b]pyridin-5-one (60 mg, 0.21 mmol) was suspended in 2.5 mL of methanol. tert-Butyl piperazine-1-carboxylate (98 mg, 0.53 mmol) was added and the reaction was heated to reflux for 8 hours. The resulting mixture was concentrated in vacuo and purified directly via flash chromatography (15-100% ethyl acetate/hexanes) to afford the title compound. 1H NMR (600 MHz, CDCl3) δ 9.79 (d, 1H); 8.49 (d, 1H); 8.22 (d, 1H); 7.77 (dd, 1H); 7.60 (d, 1H); 7.31 (d, 1H); 7.25 (d, 1H); 4.91 (dd, 1H); 3.50-3.45 (m, 4H); 2.72 (broad s, 2H); 2.63 (dd, 1H); 2.50 (dd, 1H); 2.44 (broad s, 2H); 1.46 (s, 9H). Hydroxyl proton was not observed. LRMS (APCI) calc'd for (C25H29ClN3O4) [M+H]+, 470.2; found 470.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207186B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-ee04717f981d40398c0a41e4dbbd96c7 |
| Source note | uspto-grants-2012_06 |