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Methyl 4-(benzyloxy)-5-methoxy-2-nitrobenzoate → Methyl 2-amino-4-hydroxy-5-methoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 4-(benzyloxy)-5-methoxy-2-nitrobenzoate | HCID 22667033 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 2-amino-4-hydroxy-5-methoxybenzoate | HCID 23132473 | 98.4% |
反応手順
In a 1 l Schlenk flask filled with argon, methyl 4benzyloxy-5-methoxy-2-nitrobenzoate (11.60 g, 36.6 mmol) and palladium on charcoal (1.17 g, 10% Pd, 1.1 mmol Pd) were combined and tetrahydrofuran (250 mL) was added. The argon was replaced with hydrogen (1 bar), and the mixture was vigorously stirred at r.t. until completion of the reaction. The palladium was separated by filtration through a pad of celite and the solvent was removed to obtain methyl 2-amino-4-hydroxy-5-methoxybenzoate (6.56 g, 36.0 mmol, 98%) which was used without further purification LC/ESI-MS: m/z=166 [M−CH4O+H]+; Rt=2.17 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07576090B2 |
| 出典データセット | uspto-grants-2009_08 |
| ORD ID | ord-96f0e1d9de9b48f483c376647f0bb9b6 |
| 出典メモ | uspto-grants-2009_08 |