HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67147351, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 11617178 | HCID 11617178 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67147351 | HCID 67147351 | 165.8% |
Reaction Steps
To a solution of N-(3-chlorobenzyl)-4-nitro-3-(piperazin-1-yl)benzenamine (77 mg, 0.17 mmol) in dry dichloromethane (1.0 mL) was added a saturated solution of HCl in diethyl ether (15 mL). The reaction mixture was stirred for 4 hours. The solvent was evaporated and the precipitate was recrystallized from methanol (0.3 mL), dichloromethane (0.5 mL) and diethyl ether (5 mL). The product was collected by filtration and dried in vacuo to afford the title compound (54 mg, 82% yield after recrystallization). 1H NMR (400 MHz, CD3OD): δ 8.01 (d, 1H), 7.37-7.27 (m, 4H), 6.39 (d, 1H), 6.25 (s, 1H), 4.45 (s, 2H), 3.36 (m, 4H), 3.23 (m, 4H); MS (ESI) m/z: Calculated for C17H20ClN4O2: 347.13; Observed: 347.4 (M++1) [corresponding to the free base].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968538B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-27b8c3b840d948b19b6f8f43b2597154 |
| Source note | uspto-grants-2011_06 |