HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Oxalate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 66836026 | HCID 66836026 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Oxalate | HCID 71081 | — |
| Product | HCID 66836101 | HCID 66836101 | — |
Reaction Steps
A solution of acetic acid 1-{3-[benzothiazol-2-yl(1-methylpiperidin-4-yloxy)methyl]phenyl}piperidin-4-yl ester (example 413, 100 mg) and aqueous 1N sodium hydroxide in methanol (1 mL) is stirred at room temperature for 30 min. The mixture is diluted water and extracted with dichloromethane. The pooled organic extracts are dried over magnesium sulfate and concentrated under reduced pressure. The residue is purified by chromatography (gradient dichloromethane/methanol/ammonia from 95/5/0.5 to 90/10/0.5). The base is converted into its oxalate salt in acetone to give 1-{3-[benzothiazol-2-yl(1-methylpiperidin-4-yloxy)methyl]phenyl}piperidin-4-ol, oxalate melting at 110° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029357B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-df262763719d426ba072bc06fc541e0f |
| Source note | uspto-grants-2015_05 |