化工社化工社 化学情報印刷レポート · 研究参考用
Water → Ambrisentan
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4,6-Dimethyl-2-methylsulfonylpyrimidine | HCID 2772382 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | (R)-2,4-dichlorophenylethyl ammonium (S)-2-hydroxy-3-methoxy-3,3-diphenylpropionate | HCID 86668129 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ambrisentan | HCID 6918493 | — |
反応手順
In a 25 mL three neck flask with stirring arrangement, (1 gm) (R)-2,4-dichlorophenylethyl ammonium (S)-2-hydroxy-3-methoxy-3,3-diphenylpropionate and (0.726 gm) potassium tertiary butoxide (6.488 mmol) in 10 ml DMF at 25° C. were taken and stirred for 5 min. (0.604 gm) 4,6-dimethyl-2-(methylsulfonyl)pyrimidine (3.244 mmol) was added to the reaction mixture in one lot. The reaction mixture was stirred at room temperature for 6 hours and subsequently dumped into cold water and washed the aqueous layer with toluene. Aqueous layer was collected and acidified with HCl to pH 2. The solid was extracted with ethyl acetate, and wash the ethyl acetate layer with water followed by brine. Dry over sodium sulphate and concentrated on Buchi Rotavapor.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08962832B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-cfa0838c16104336aac10dcfe2d00eec |
| 出典メモ | uspto-grants-2015_02 |