HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 67749524, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 67749549 | HCID 67749549 | — |
| Solvent | Hydrogen Bromide | HCID 260 | — |
| Product | HCID 67749524 | HCID 67749524 | 64% |
Reaction Steps
A solution of 0.57 g (2.0 mmol) methoxy-amine cis(±)-1,2,3,4-tetrahydro-8-methoxy-N,1-di-propyl-2-naphthalenamine hydrochloride in 10 mL 48% hydrobromic acid was refluxed (bath temperature, 120° C.) for eight hours. TLC analysis showed no starting material remaining. The mixture was cooled to room temperature, treated with 20% sodium hydroxide to pH 7-8, and extracted with ethyl acetate. The organic layer was washed with brine, dried (MgSO4), filtered, and concentrated in vacuo. The oil was converted to HCl-salt with excess anhydrous hydrochloric acid and recrystallized from ethyl acetate to give 0.36 g (64%) of pure title compound as a white solid: m.p. 244°-245° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06331636B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-852735b805744b889ef94f259ac49ec4 |
| Source note | uspto-grants-2001_12 |