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3-(2-Aminoethyl)phenol hydrochloride → Ethyl 6-hydroxy-1,2,3,4-tetrahydroisoquinoline-1-carboxylate hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-(2-Aminoethyl)phenol hydrochloride | HCID 77001 | — |
| 反応物 | Ethyl glyoxylate toluene | HCID 86599969 | — |
| 溶媒 | Toluene ethanol | HCID 21863594 | — |
| 生成物 | Ethyl 6-hydroxy-1,2,3,4-tetrahydroisoquinoline-1-carboxylate hydrochloride | HCID 19865448 | 90.1% |
反応手順
A solution of 3-(2-aminoethyl)phenol hydrochloride (4.60 g, 26.49 mmol) and 47% ethyl glyoxylate/toluene solution (polymer form) (6.15 mL, 29.14 mmol) in a mixed solvent of toluene/EtOH (50 mL) was heated under reflux for 18 hr. The reaction mixture was concentrated under reduced pressure. The precipitate was collected by filtration, and washed with ethyl acetate/diethyl ether to give ethyl 6-hydroxy-1,2,3,4-tetrahydroisoquinoline-1-carboxylate hydrochloride (6.15 g, 23.86 mmol, 90%) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09365520B2 |
| 出典データセット | uspto-grants-2016_06 |
| ORD ID | ord-53a8838a2c164503a4106c4f49a4b39a |
| 出典メモ | uspto-grants-2016_06 |