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Hydrochloric Acid → HCID 178501122、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 2-Nitrobenzeneacetaldehyde | HCID 10844764 | — |
| 反応物 | HCID 178501119 | HCID 178501119 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178501122 | HCID 178501122 | 27% |
反応手順
A solution of (2-Nitro-phenyl)-acetaldehyde (1 g, 5.98 mmol), trans-4-Aminomethyl cyclohexanecarboxylic acid methyl ester hydrogen chloride salt (1.37 g, 6.58 mmol) and TEA (0.92 mL, 6.58 mmol) in dry DCM was stirred at room temperature for 2.5 h. Sodium triacetoxy borohydride (2.53 g, 11.96 mmol) was added and the mixture stirred at room temperature for 25 min. Then (2N) HCl was added until acidic pH and the aqueous layer extracted with DCM. The organic layer was washed with a saturated solution of NaHCO3 and dried over Na2SO4 anhydrous and then evaporated to afford crude product. Finally, the crude product was purified by flash chromatography on silica (ETP/EtOAc 9/1→0/1) to obtain the titled compound (0.51 g, yield: 27%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865704B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-46d4c2e571d7477b818f60875b53b2d1 |
| 出典メモ | uspto-grants-2014_10 |