HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → 2-(4-(Bis(4-chlorophenyl)methyl)-2-oxopiperazin-1-yl)acetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | Methyl 2-(4-(bis(4-chlorophenyl)methyl)-2-oxopiperazin-1-yl)acetate | HCID 68928666 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | 2-(4-(Bis(4-chlorophenyl)methyl)-2-oxopiperazin-1-yl)acetic acid | HCID 25063692 | 88% |
Reaction Steps
To a solution of methyl 2-(4-(bis(4-chlorophenyl)methyl)-2-oxopiperazin-1-yl)acetate (160 mg, 393 μmol) in THF/MeOH/H2O=5:5:1 (5.5 mL) was added lithium hydroxide monohydrate (49.5 mg, 1.179 mmol) and the resulting solution was stirred overnight. The solvent was evaporated, diluted with water, adjusted to pH=5 with 10% HCl, extracted with DCM, dried over Na2SO4, filtered and evaporated to dryness under high vacuum. The residue was loaded onto flash column (SiO2, DCM to DCM/MeOH=100:5 to 100:10 to 100:15 to 100:20) to give 2-(4-(bis(4-chlorophenyl)methyl)-2-oxopiperazin-1-yl)acetic acid (136 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08183244B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-fae8d5f20a634126b6fc590acfb0e08a |
| Source note | uspto-grants-2012_05 |