関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | (RS)-2-amino-3-(8-ethyl-naphthalen-1-yl)-propionitrile | HCID 57543207 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(8-Ethyl-naphthalen-1-yl)-propane-1,2-diamine | HCID 57543199 | 28.2% |
反応手順
A suspension of LiAlH4 (117 mg) in THF (2 ml) was cooled to 0° C. and treated under an argon atmosphere with a solution of (RS)-2-amino-3-(8-ethyl-naphthalen-1-yl)-propionitrile (230 mg) in THF (4 ml). The reaction mixture was stirred for 5 hrs at r.t., then treated sequentially at 0° C. with 0.1 ml H2O, 0.1 ml 4N NaOH and 0.5 ml H2O. After stirring for 30 min, the solid was filtered off and washed with THF. The filtrate was concentrated. The crude product was isolated by column chromatography (silica gel; eluent: CH2Cl2→CH2Cl2/MeOH 9:1) to give 3-(8-ethyl-naphthalen-1-yl)-propane-1,2-diamine (66 mg) as light brown oil. MS (ISP): 229.3 ((M+H)+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07812047B2 |
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| 出典データセット | uspto-grants-2010_10 |
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| ORD ID | ord-a09cb40fce2e47bc9bbdc71fc9fed21a |
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| 出典メモ | uspto-grants-2010_10 |
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