HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic 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 methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| 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 | Ethyl Acetate | HCID 8857 | — |
| 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 methanesulfonate | HCID 86677401 | — |
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 (Example 6f, 50 mg) was dissolved in ethyl acetate (5 mL), and a solution of methanesulfonic acid (0.0041 mL) in ethyl acetate (0.5 mL) was added dropwise thereto. The resulting mixture was stirred overnight at room temperature, and the precipitated solid was filtered. The filtrate obtained was washed with ethyl acetate and TBME, and dried. The captioned compound (48 mg) was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436009B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-55d1ba8773034d909b491aaca936c356 |
| Source note | uspto-grants-2013_05 |