HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18617602, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 18617476 | HCID 18617476 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 18617602 | HCID 18617602 | 88% |
Reaction Steps
Ethyl 4-(6-oxo-piperidin-3-yl)-benzoate (320 mg, 1.30 mmol, reference example 66) is dissolved in MeOH (8 mL). To this solution is added 1 N NaOH (1.43 mL, 1.43 mmol) and the resulting solution stirred at room temperature for 1 hour. An additional portion of 1 N NaOH (2 mL) is added and the mixture allowed to stir at room temperature overnight (16 hours). 1 N HCl is added until pH 2-3 is reached. A precipitate formed and is filtered, washed with water and placed in a vacuum oven to dry overnight to afford the title compound (250 mg, 88%) as small white crystals (needles). 1H NMR (300 MHz, DMSO) δ 1.94 (m, 2H), 2.23 (m, 2H), 3.06 (m, 1H), 3.23 (m, 2H), 7.42 (d, J=8.3, 2H), 7.57 (bs, 1H), 7.87 (d, J=8.1, 2H); MS (Ion spray) m/z 220 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06541505B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-c62f37d8430d494f84cf10f44f5244a2 |
| Source note | uspto-grants-2003_04 |