HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 50898963, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 87181084 | HCID 87181084 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 50898963 | HCID 50898963 | 48.8% |
Reaction Steps
A mixture of EXAMPLE 17A (40.0 mg, 0.082 mmol) and 20% sodium hydroxide (0.1 mL) in dioxane (1.5 mL) was heated at 50° C. for 2 h. The mixture was concentrated and the residue treated with water, sonicated, filtered, and washed with water. The solids were dissolved in 6 mL hot 1:1 dimethylsulfoxide/methanol. After cooling, a precipitate formed and additional methanol was added. The solids were filtered, washed with methanol, and dried to give 14.0 mg (32%) of the title compound. 1H NMR (300 MHz, DMSO-D6) 7.41-7.67 (m, 3H), 7.95-8.16 (m, 3H), 8.39 (d, J=2.4 Hz, 1H), 8.60 (d, J=2.8 Hz, 1H), 8.77 (s, 1H), 9.08 (d, J=1.2 Hz, 1H), 10.98 (s, 1H), 12.74 (s, 1H). MS (ESI) m/z 350.5 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08383624B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-2bcdd7cc31c7422aacd25ca972dacf65 |
| Source note | uspto-grants-2013_02 |