HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → [(4-Fluoro-phenyl)-methyl-amino]-phenyl-acetic acid hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | Ethyl 2-((4-fluorophenyl)(methyl)amino)-2-phenylacetate | HCID 58556946 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | [(4-Fluoro-phenyl)-methyl-amino]-phenyl-acetic acid hydrochloride | HCID 67124664 | 72% |
Reaction Steps
To a solution of [(4-fluoro-phenyl)-methyl-amino]-phenyl-acetic acid ethyl ester (I70) (0.59 g, 2.05 mmol) in THF (10 mL) and water (10 mL), is added lithium hydroxide hydrate (0.26 g, 6.14 mmol). The reaction is stirred at RT for 3.5 hours and then at 70° C. for 24 hours. 3N HCl is added till pH is about 1 and the mixture is evaporated. Water (15 mL) is added and the residue is triturated obtaining a pale brown suspension that is filtered on a buckner funnel, washed with water and then with acetonitrile. The solid is dried under vacuum at 40° C. overnight to obtain intermediate I119 as a pale brown powder (0.44 g, 72% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835682B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-033bd5ca5b0d47be8c534378e1c883d4 |
| Source note | uspto-grants-2014_09 |