HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68998787, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 69049137 | HCID 69049137 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68998787 | HCID 68998787 | 90% |
Reaction Steps
To a 20 mL vial which contained a solution of the product from step 3 (21 mg, 0.05 mmol) in dioxane (1 mL) was added HCl (4 N in dioxane, 2 mL) at 0° C. The mixture was allowed to warm to rt and stirred at rt for 16 h. The solvent was reduced to 1 mL and ether (15 mL) was added to this vial. The resulting solid was filtered out and dried in vacuo to yield the title product (15 mg, 90%); LCMS); 87%, ESI+, Calcd. 309.4. Found m/z 310.5 (M+1). 1H NMR (400 MHz, DMSO-d6); δ 1.66-1.79 (m, 1H), 1.84-2.05 (m, 2H), 2.05-2.18 (m, 1H), 3.17-3.28 (m, 2H), 3.97-4.07 (m, 1H), 4.11-4.18 (m, 1H), 4.29 (dd, J1=10.4 Hz, J2=3.2 Hz, 1H), 6.69-6.73 (m, 1H), 6.80-6.83 (m, 1H), 7.06-7.11 (m, 3H), 7.33-7.38 (m, 3H):
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07402684B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-cfe42f8387764ce6b7230802726cfbc1 |
| Source note | uspto-grants-2008_07 |