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4-Amino-3-hydroxypyridine → N,N-Diethyl-N'-(3-hydroxypyridin-4-yl)methanimidamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Amino-3-hydroxypyridine | HCID 2762419 | — |
| 反応物 | N-(Dimethoxymethyl)-N-ethylethanamine | HCID 12747026 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N,N-Diethyl-N'-(3-hydroxypyridin-4-yl)methanimidamide | HCID 15380930 | 61.5% |
反応手順
A mixture of 4-amino-3-pyridinol (3.90 g), N,N-diethylformamide dimethyl acetal (11.68 g) and toluene (20 mL) was heated under nitrogen for 2 hours. The solution was concentrated under reduced pressure. The resulting liquid was filtered through silica gel with 10% ethanol in tetrahydrofuran to give a solid. Recrystallization of the purified product from ethyl acetate/hexanes afforded 4.21 g of crystalline solid, m.p. 104°-106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05821239 |
| 出典データセット | uspto-grants-1998_10 |
| ORD ID | ord-ab203fee87d3404db4af9fdffee41eee |
| 出典メモ | uspto-grants-1998_10 |