関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Tert-butoxycarbonyl-1,2,3,4-tetrahydrobenzo[b]thieno[2,3-c]pyridine-carboxylic acid ethyl ester | HCID 19960856 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Tert-butoxycarbonyl-1,2,3,4-tetrahydro-benzo[b]thieno[2,3-c]pyridine-3-carboxylic acid | HCID 69959606 | 75% |
反応手順
In a mixed solvent of 30 ml of methanol and 20 ml of chloroform was dissolved 6 g of 2-tert-butoxycarbonyl-1,2,3,4-tetrahydrobenzo[b]thieno[2,3-c]pyridine-carboxylic acid ethyl ester and 4 ml of an aqueous solution of 5N sodium hydroxide was further added thereto, and then the solution was refluxed for 5 hours. The solvents were distilled off under reduced pressure and 300 ml of 5% citric acid and 300 ml of chloroform were added to the residue. The chloroform layer was washed with a saturated aqueous sodium chloride solution and then dried by sodium sulfate. After distilling off chloroform under reduced pressure, the residue formed was recrystallized from a mixture of chloroform and hexane to provide 4.15 g (yield of 75%) of 2-tert-butoxycarbonyl-1,2,3,4-tetrahydrobenzo[b]thieno[2,3-c]pyridine-3-carboxylic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05126448 |
|---|
| 出典データセット | uspto-grants-1992_06 |
|---|
| ORD ID | ord-36cccc27ee4145db9b1c284e496830da |
|---|
| 出典メモ | uspto-grants-1992_06 |
|---|