HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69433929, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 11437893 | HCID 11437893 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69433929 | HCID 69433929 | — |
Reaction Steps
The product of Example 12B (50 mg, 0.17 mmol) in ethyl acetate (5 mL) was treated with 4M HCl in 1,4-dioxane (0.2 mL, 0.8 mmol) at ambient temperature for 10 hours. The title compound was obtained as a solid (30 mg, yield, 44%). 1H NMR (MeOH-d4, 300 MHz) δ 1.90-2.25 (m, 3H), 2.30-2.45 (m, 1H), 2.70-2.76 (m, 1H), 3.37-3.52 (m, 5H), 3.90-3.98 (m, 1H), 5.42-5.50 (m, 1H), 6.71 (s, 2.5H), 6.81-6.89 (m, 1H), 7.03 (d, J=8.9 Hz, 1H), 7.41 (ddd, J=7.8, 2.4, 1.0 Hz, 1H), 7.60-7.68 (m, 2H), 7.75 (dt, J=7.8, 1.0 Hz, 1H), 8.05 (dd, J=8.8, 2.7 Hz, 1H), 8.45 (d, J=2.7 Hz, 1H) ppm. MS (DCl/NH3) m/z 296 (M+H)+. Anal. Calculated for C18H21N3O.3.3HCl.1.0H2O: C, 49.85; H, 6.11; N, 9.69. Found: C, 49.93; H, 5.77; N, 9.51.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07309699B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-821e4c4c2a664affbe2a3a82dc1068f1 |
| Source note | uspto-grants-2007_12 |