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Hydrochloric Acid → Tetrahydrothiopyran-4-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Thiane-4-carbonitrile | HCID 21598641 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Tetrahydrothiopyran-4-carboxylic acid | HCID 21598642 | 60% |
反応手順
A solution of 1.97 g (15.5 mmol) of tetrahydro-thiopyran-4-carbonitrile in 5 mL of ethanol (EtOH) was added to a solution of 6.2 g (155 mmol) of sodium hydroxide (NaOH) in 30 mL of EtOH and 15 mL of water, and the resulting mixture was heated at reflux for 4 h. The reaction mixture was cooled in an ice bath, acidified with concentrated hydrochloric acid to pH=2, and then concentrated to give a precipitate which was filtered to afford 1.36 g (60%) of desired tetrahydro-thiopyran-4-carboxylic acid as a brown crystalline solid as indicated by 1H NMR.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07196111B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-7dece2fd7d37467bbf55b4ed9dc15e04 |
| 出典メモ | uspto-grants-2007_03 |