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Methanesulfonic Acid → 3-(2-Hydroxyethyl)-5-(1,2,4-triazol-1-ylmethyl)-1h-indol-2-carboxylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 3-(2-Hydroxyethyl)-5-[1,2,4]triazol-1-ylmethyl-1h-indol-2-carboxylic acid | HCID 10356643 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(2-Hydroxyethyl)-5-(1,2,4-triazol-1-ylmethyl)-1h-indol-2-carboxylic acid methyl ester | HCID 11630801 | 93.6% |
反応手順
2.7 ml (42 mmoles) of methanesulphonic acid were added to a suspension de 6 g (21 mmoles) of the 3-(2-hydroxyethyl)-5-[1,2,4]triazol-1-ylmethyl-1H-indol-2-carboxylic acid in 120 ml of methanol. The mixture was left under stirring at reflux temperature for 3 hours. The solvent was evaporated to dryness under reduced pressure, the residue dissolved with 20 ml of a saturated bicarbonate solution and extracted 3 times with ethyl acetate. The combined organic phases were dried and evaporated to dryness, and the evaporated solid recrystallised from isopropyl alcohol/heptane to give 5.9 g (93%) of the title ester as a yellow crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07279581B2 |
| 出典データセット | uspto-grants-2007_10 |
| ORD ID | ord-808bd576f9724ea895b7e69c75fc2e71 |
| 出典メモ | uspto-grants-2007_10 |