HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66792826, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 66792833 | HCID 66792833 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 66792826 | HCID 66792826 | 64% |
Reaction Steps
To a stirring solution of methyl (2-{[4-(2-tert-butylphenyl)piperazin-1-yl]carbonyl}-5-oxopyrrolidin-1-yl)acetate obtained in Example 64 (0.39 g, 0.97 mmol) in methanol (12 mL) was added 1 M lithium hydroxide (2.9 mmol, 2.9 mL) and the mixture was stirred at room temperature for 1 h. The reaction mixture was acidified with 1 M hydrochloric acid (pH 3) and concentrated under reduced pressure. The resulting residue was partitioned between ethyl acetate and water, and the organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting solid was recrystallized from hexane-diethyl ether to give the title compound (0.24 g, 64%) as a white solid, mp 273° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853215B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-0cd458175adf49f19ec30532f4e2d9ea |
| Source note | uspto-grants-2014_10 |