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Stannous chloride dihydrate → 2-Amino-4-(benzyloxy)-5-methoxybenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 4-(Benzyloxy)-5-methoxy-2-nitrobenzoic acid | HCID 10859633 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Amino-4-(benzyloxy)-5-methoxybenzoic acid | HCID 10967675 | — |
反応手順
A solution of 4-benzyloxy-5-methoxy 2-nitrobenzoic acid (18.18 g, 60 mmol)(D. E. Thurston et al., Synthesis (1990), 81) and SnCl2.2H2O (137 g, 0.6 mol) (Showa Chemical Company, Japan) in MeOH (800 mL) was stirred at 70° C. for 5 h. The mixture was concentrated under vacuum to a thick syrup. Ethyl acetate (300 mL) was then added. The organic phase was washed with water until it turned to a clear solution, then washed with brine, and dried over MgSO4. After removal of solvent, the crude was recrystallized from ethyl acetate to obtain the title compound in the form of a yellow solid with a yield of 15.1 g (92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06660856B2 |
| 出典データセット | uspto-grants-2003_12 |
| ORD ID | ord-87f565170a074cf9858bf3687fb98661 |
| 出典メモ | uspto-grants-2003_12 |