HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 118235798, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 118235620 | HCID 118235620 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118235798 | HCID 118235798 | 72.2% |
Reaction Steps
To a solution of Example 311 (0.219 g, 0.358 mmol) in THF (4 mL) was added lithium hydroxide monohydrate (0.03 g, 0.716 mmol) and the mixture was stirred at room temperature for 4 h. The pH of the mixture was adjusted to ˜6 by the dropwise addition of a 10% aqueous solution of citric acid. The material was concentrated in vacuo, and the residue was washed with acetone, to furnish the title compound (0.135 g, 72%). δH (300 MHz, DMSO-d6) 8.57 (m, 3H), 7.66 (m, 1H), 7.51 (m, OH), 7.41 (dd, OH, J 9.3, 1.5 Hz), 7.23 (m, 1H), 7.09 (m, 2H), 6.99 (m, OH), 5.31 (m, OH), 3.95 (d, 4H, J 3.9 Hz), 3.20 (m, 2H), 2.25 (s, 3H). LCMS (pH 10): MH+ 523.2, RT 1.05 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09309243B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-7deec16a4e58478287a0f8a314fcc456 |
| Source note | uspto-grants-2016_04 |