HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22272563, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Tert-butyl 1,4-diazepane-1-carboxylate | HCID 2756058 | — |
| Reactant | HCID 22272449 | HCID 22272449 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 22272563 | HCID 22272563 | — |
Reaction Steps
N-(5-Fluoro-2-nitrophenyl)-N-methylmethanesulfonamide (3.1 g, 12.5 mmol), tert-butyl 1-homopiperazinecarboxylate (2.5 g) and potassium carbonate (2 g) were heated together in DMSO (50 mL) at 80° C. overnight. The solution was allowed to cool and poured into 500 mL of water. The solid product was collected by filtration, washed with water and dried. Yield 4.6 g (86%); 1H NMR (400 MHz, CDCl3) δ 1.41 (s, 9H), 2.0 (br s, 2H), 3.01 (s, 3H), 3.28 (s, 3H), 3.3–3.8 (br, 8H), 6.64 (d, J=8.1 Hz, 1H), 6.74 (d, J=4.8 Hz, 1H), 8.09 (d, J=8.1 Hz, 1H); MS (ESI+) for C18H28N4O6S m/z 428.1709 (M+) (calc. 428.173).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07173035B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-12ab65fe86e4433da1683fffb03382cd |
| Source note | uspto-grants-2007_02 |