HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22596838, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 22596830 | HCID 22596830 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22596838 | HCID 22596838 | 72.8% |
Reaction Steps
A solution of methyl 3-fluoro-4-[3-pentyl-3-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-ureido]-benzoate (17 mg) in 10 mL THF/3 mL methanol/3 mL water was treated with lithium hydroxide hydrate (20 mg). The mixture was stirred at room temperature for two hours. The mixture was diluted with 5 mL water and the pH was adjusted to 2 with conc. HCl. The mixture was extracted with three 10 mL portions of ether. The combined organic extracts were dried over MgSO4, filtered and concentrated in vacuo, giving a brown solid. The product was purified by trituration in hexanes, yielding 12 mg 3-fluoro4-[3-pentyl-3-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-ureido]-benzoic acid as a yellow solid. M.P. 151-157° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06844466B2 |
| Source dataset | uspto-grants-2005_01 |
| ORD ID | ord-d7f20c75f62e4df983e92e24f5df3772 |
| Source note | uspto-grants-2005_01 |