HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen chloride-ethyl acetate → N-[1-(phenylaminocarbonylmethyl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | N-[1-(phenylaminocarbonylmethyl)-piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide | HCID 70246692 | — |
| Solvent | Chloroform methanol | HCID 21584188 | — |
| Product | N-[1-(phenylaminocarbonylmethyl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride | HCID 70248335 | 60% |
Reaction Steps
To a solution of N-[1-(phenylaminocarbonylmethyl)-piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in chloroform-methanol (1:1) was added 2 ml (8.0 mM) of 4N-HCl/ethyl acetate. The solvent was distilled off under reduced pressure and the residue was diluted with ethanol/ether ({fraction (1/10)}). The resulting crystals were collected by filtration and rinsed with ethanol and diethyl ether to provide the title compound as orange-colored crystals (506 mg, 60%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06235731B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-fc229b3bdf074c29872b73ff96cc0563 |
| Source note | uspto-grants-2001_05 |