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1-Propanesulfonic 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 propanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Propanesulfonic acid | HCID 78938 | — |
| 反応物 | 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 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 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 propanesulfonate | HCID 86677406 | — |
反応手順
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, 100 mg) was dissolved in ethyl acetate (10 mL), a solution of 1-propanesulfonic acid [CAS No. 5284-66-2] (13.5 mg) in ethyl acetate (1 mL) was added dropwise thereto. The resulting mixture was stirred at room temperature for 22 hours, and the precipitated solid was filtered. The solids recovered by filtration were washed with ethyl acetate and TBME, and dried. The captioned compound (90 mg) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08436009B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-2e44d4a1045040d58a204d93b19e7e9b |
| 出典メモ | uspto-grants-2013_05 |