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Hydrochloric 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 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 6-(1,2,4-Triazol-1-ylmethyl)-4,9-dihydro-3h-pyrano[3,4-b]indol-1-on | HCID 10400822 | — |
| 生成物 | 3-(2-Hydroxyethyl)-5-(1,2,4-triazol-1-ylmethyl)-1h-indol-2-carboxylic acid methyl ester | HCID 11630801 | 94% |
反応手順
To a suspension of 2.5 g (8.2 mmoles) of the 6-(1,2,4-triazol-1-ylmethyl)-4,9-dihydro-3H-pyrano[3,4-b]indol-1-on a hydrochloride in 50 ml of methanol were added 0.66 ml (10.2 mmoles) of methanesulphonic acid. The mixture was left under stirring at the reflux temperature for 4 hours. The solvent was evaporated to dryness under reduced pressure, the residue dissolved with 10 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 2.3 g (94%) 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-7696ed5722304a4fb55c267a2688eea7 |
| 出典メモ | uspto-grants-2007_10 |