関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 1-methyl-1H-indole-5-carbaldehyde | HCID 7537534 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | n-Methyl-1-(1-methyl-1h-indol-5-yl)methanamine | HCID 18525753 | 45% |
反応手順
1-Methyl-1H-indole-5-carbaldehyde (338 mg, 2.13 mmol) was dissolved in anhydrous methanol (10 ml). Methylamine (0.80 ml of 33% solution in ethanol, 6.43 mmol) was added and the reaction was stirred for 3 h. The solution was concentrated to a brown oil and then dissolved in anhydrous methanol (10 ml). Sodium borohydride (83.0 mg, 2.19 mmol) was added and the mixture was stirred overnight at room temperature. Water (4 ml) was added and the solution was concentrated. Sodium hydroxide (8 ml, 1N) was added and the aqueous layer was extracted with ethyl acetate (3×20 ml). Combined organic layers were dried over MgSO4, filtered and concentrated to afford methyl-(1-methyl-1H-indol-5-ylmethyl)-amine (167 mg, 45%) as an orange oil: 1H NMR (400 MHz, DMSO-d6) δ 7.44 (s, 1H), 7.34 (d, J=8.0 Hz, 1H), 7.261 (d, J=3.2 Hz, 1H), 7.11 (d, J=12.0 Hz, 1H), 6.345 (d, J=4.0 Hz, 1H), 3.75 (s, 3H), 3.70 (s, 2H), 2.25 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07879872B2 |
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| 出典データセット | uspto-grants-2011_02 |
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| ORD ID | ord-00c2ad85f56b4055a48316a99d331c20 |
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| 出典メモ | uspto-grants-2011_02 |
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