HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68875089, compound → HCID 68872386, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68875089 | HCID 68875089 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68872386 | HCID 68872386 | 83% |
Reaction Steps
A solution of Example 55E (0.055 g, 0.174 mmol) in 4 mL of dioxane and 4 mL of 1N HCl was refluxed for 3 hours. The solution was cooled to room temperature, diluted with water and extracted with 3× ethyl acetate. The combined organic layers were dried over MgSO4, and concentrated in vacuo to yield the title compound (0.035 g, 83% yield) as an oil that solidifies on standing. 1H NMR (300 MHz, DMSO-d6): δ ppm 1.16 (m, 3H) 1.48 (s, 3H) 1.70 (m, 3H) 2.04 (m, 2H) 2.21 (m, 1H) 5.76 (m, 1H) 7.30 (m, 1H) 7.44 (m, 1H) 7.63 (m, 1H) 8.00 (d, J=8.09 Hz, 1H). MS (ESI+) m/z=243 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07538105B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-4401da4d75b841fda946778fd9c9c272 |
| Source note | uspto-grants-2009_05 |