関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chloro-2-nitrobenzaldehyde | HCID 79674 | — |
| 反応物 | 1-Boc-3-aminopyrrolidine | HCID 2756370 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 66758130 | HCID 66758130 | — |
反応手順
To a solution of 3-Amino-pyrrolidine-1-carboxylic acid tert-butyl ester (2 g, 10.7 mmol) in methanol (20 mL) was added 4-Chloro-2-nitro-benzaldehyde (1.98 g, 10.7 mmol). The resultant solution was heated at 60° C. overnight. The reaction mixture was cooled to 0° C. and to it was added NaBH4 (629 mg, 10 mmol). After 1 h, the reaction solution was quenched with saturated NaHCO3 solution and extracted with ethyl acetate. The organic extract was dried over MgSO4, filtered and concentrated to provide the crude product as an oil. The crude product was used in the subsequent reaction without further purification. LCMS (retention time=1.28, ES+; 356)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653096B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-816b0c49c9614adb8740b35af458b82f |
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| 出典メモ | uspto-grants-2014_02 |
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