HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanesulfonic acid → 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]-triazol-3-yloxymethyl ester ethanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanesulfonic acid | HCID 11668 | — |
| Reactant | 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester | HCID 67471184 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]-triazol-3-yloxymethyl ester ethanesulfonate | HCID 86677405 | 87% |
Reaction Steps
At room temperature, 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester (1.0 g, 1.28 mmol) was dissolved in acetone (80 mL), and a solution of ethanesulfonic acid (127 mg, 1.15 mmol) in acetone (20 mL) was added dropwise thereto. To the resulting mixture, a seed crystal of the captioned compound was added, and the resulting mixture was stirred overnight at room temperature. The precipitated solid was filtered, washed with acetone, and then dried to obtain the captioned compound (889 mg) as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436009B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-cdb52189ea2d4ff693cd8167b0b24374 |
| Source note | uspto-grants-2013_05 |