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Sodium cyanoborohydride → [2-(3-Fluoro-4-nitro-phenyl)-ethyl]-dimethyl-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | [2-(3-Fluoro-4-nitro-phenyl)-vinyl]-dimethyl-amine | HCID 91252016 | — |
| 触媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | [2-(3-Fluoro-4-nitro-phenyl)-ethyl]-dimethyl-amine | HCID 118024700 | 63.6% |
反応手順
To a solution of [2-(3-fluoro-4-nitro-phenyl)-vinyl]-dimethyl-amine (1.7 g, 8 mmol) in MeOH, was added NaBH3CN (770 g, 12 mmol) and one drop of AcOH. The reaction mixture was stirred at room temperature for 2 hours and quenched with water. After removal of all volatiles in vacuo, the residue was extracted with 10% methanol in DCM twice. The combined extracts were washed with brine, dried over anhydrous sodium sulfate. Concentration under vacuum gave a crude product, which was purified by reverse phase column to afford the title compound (1.08 g, yield: 63%). MS (ESI): 213 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434697B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-c800bd55957a40af80233547b65c2632 |
| 出典メモ | uspto-grants-2016_09 |