HuagongsheHuagongshe Chemistry Print Report · For research reference only
CJ-040714 → N-({1-[(4-Hydroxytetrahydro-2H-pyran-4-yl)methyl]piperidin-4-yl}methyl)-3-isopropyl-2-oxo-2,3-dihydro-1H-benzimidazole-1-carboxamide hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | CJ-040714 | HCID 11350913 | — |
| Reactant | Hydrochloride methanol | HCID 21893726 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | N-({1-[(4-Hydroxytetrahydro-2H-pyran-4-yl)methyl]piperidin-4-yl}methyl)-3-isopropyl-2-oxo-2,3-dihydro-1H-benzimidazole-1-carboxamide hydrochloride | HCID 68459910 | 90% |
Reaction Steps
To a stirred solution of N-({1-[(4-hydroxytetrahydro-2H-pyran-4-yl)methyl]piperidin-4-yl}methyl)-3-isopropyl-2-oxo-2,3-dihydro-1H-benzimidazole-1-carboxamide (27.0 g, 62 mmol) in methanol (150 mL) was added 10% HCl-methanol (100 mL) at ambient temperature. After 30 min, the volatile materials were removed by evaporation. The resulting amorphous was precipitated by ethanol/diethylether. The precipitate was recrystallized from ethanol/diethylether (1:1) to give 26.5 g (90%) of title compound as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776885B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-bca344ea65d54d10b2f0a28c5ec3cff6 |
| Source note | uspto-grants-2010_08 |