HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86696276, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86696274 | HCID 86696274 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86696276 | HCID 86696276 | 39.8% |
Reaction Steps
The crude (77.2) was dissolved in THF (20 ml) and 1 ml of HCl (2N) was added. The mixture was stirred at rt for 10 min. The mixture was neutralized by saturated aqueous NaHCO3 and evaporated to dryness. The residue was purified by column chromatography (CombiFlash-ISCO, eluent DCM/MeOH from 20/1 to 8/1 for 40 min gradiently) to afford the title compound (40 mg, yield 39.8% over 2 steps). LCMS (method A): [M+H]+=405.6, tR=2.08 min. 1H NMR (400 MHz, CDCl3) δ ppm 2.57 (s., 3H) 3.17-3.34 (t, 4H) 3.82-4.00 (t, 4H) 7.15 (d, 1H) 7.46 (d, 1H) 7.64 (s, 1H) 7.88 (s, 2H) 7.93 (d, 1H) 8.76 (d, 1H) 8.78 (s, 1H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062045B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-8d786eaa7e0541e692ebf2f6b601f55f |
| Source note | uspto-grants-2015_06 |