HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide | HCID 66618074 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide hydrochloride | HCID 66618073 | 194.3% |
Reaction Steps
3 M hydrochloric acid (9.2 ml, 27.8 mmol) was added dropwise to an ethanol (200 ml) suspension of 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (5446.6 mg, 11.6 mmol) at 25° C., while the suspension was stirred. The resulting mixture was stirred for 3.5 hours. The obtained crystal was collected by filtration, was then washed with ethanol (50 ml), and was then dried under reduced pressure at 40° C. for 14 hours, so as to obtain the above title compound (5436.1 mg, 116. mmol). Yield: 99%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08815880B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-670d00eeee6f4f4b8a37dda5572fbe26 |
| Source note | uspto-grants-2014_08 |