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Stannous chloride dihydrate → 3-Aminocinnamic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | Ethyl-m-nitrocinnamate | HCID 94827 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Aminocinnamic acid ethyl ester | HCID 97825 | — |
反応手順
Ethyl 3-nitrocinnamate (1) (2.0 g, 9.04 mmol) was reduced using method A, except that SnCl2.2H2O (10.2 g, 45.20 mmol) in EtOH (20 mL) was used and after the reaction the solvent was concentrated in vacuo, Rochelle's salt and saturated NaHCO3 (1:1, 80 mL) were added, and the aqueous basified with 1N NaOH. The aqueous was extracted with EtOAc (3×40 mL), washed with Rochelle's salt/saturated NaHCO3 solution (2×40 mL), dried (MgSO4) and the solvent was concentrated in vacuo to give the title compound. Yield: 1.77 g, >100%; LC/MS tr 0.89 min; MS (ES+) m/z 192 (M+H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08080567B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-5b0e7255ce0e49e88ae40a507b94bae2 |
| 出典メモ | uspto-grants-2011_12 |