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N-Methylbutylamine → 4-[[(N-methyl-N-butylamino)methylene]amino]-3-pyridinol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-Methylbutylamine | HCID 8068 | — |
| 反応物 | Ammonium Sulfate | HCID 6097028 | — |
| 反応物 | 4-[[(Dimethylamino)methylene]amino]-3-pyridinol | HCID 15380929 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-[[(N-methyl-N-butylamino)methylene]amino]-3-pyridinol | HCID 15380936 | 64.2% |
反応手順
A mixture of 4-[[(dimethylamino)methylene]amino]-3-pyridinol (7.50 g), N-methylbutylamine (8.10 g), ammonium sulfate (0.600 g), and anhydrous toluene (25 mL) was heated at reflux under nitrogen for 2.25 hours. The solution was concentrated under reduced pressure and the crude product chromatographed on silica gel (10% methanol in dichloromethane) to afford 6.04 g of solid. Recrystallization from ethyl acetate/hexanes afforded 3.90 g of a crystalline material, m.p. 83°-85° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05869480 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-c9b102cdfcab4b2b80f20526c9c4c03c |
| 出典メモ | uspto-grants-1999_02 |