HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69084156, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 69280794 | HCID 69280794 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 69084156 | HCID 69084156 | 118.5% |
Reaction Steps
A solution of 159 (150 mg, 0.16 mmol) in methanol (10 mL) was treated with concentrated aqueous HCl (1 mL) for 1 hour at room temperature, then the resulting solution was concentrated under vacuum to give a residue, which was dissolved into methanol (5 mL) and neutralized with concentrated NH4OH (1 mL). After removal of all the solvent, the residue was purified by flash column chromatography with 10% methanol in dichloromethane to afford the title compound as a white solid (50.1 mg, 38%). (ES, m/z); [M+H]+ 265.0; 1H NMR (300 MHz, D2O) δ 6.23 (d, J=6.6 Hz, 1H), 4.97-4.70 (m, 1H), 4.22-4.19 (m, 1H), 4.02-3.99 (m, 1H), 3.67-3.62 (m, 2H), 2.91 (s, 6H), 1.26 (dd, J=6.6 Hz, 26.1 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901087B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-53333fd5383947b6b43bcf3d6546a1c3 |
| Source note | uspto-grants-2014_12 |