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4-Amino-3-hydroxypyridine → 4-[[(Diisopropylamino)methylene]amino]-3-pyridinol
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 | Diisopropylformamide Dimethylacetal (>90%) | HCID 13161384 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-[[(Diisopropylamino)methylene]amino]-3-pyridinol | HCID 15380931 | — |
反応手順
A mixture of 4-amino-3-pyridinol (3.0 g), N,N-diisopropylformamide dimethyl acetal (9.54 g) and 15 ml dry toluene was stirred at room temperature for 18 hours and thereafter heated to 60°-70° C. After 90 minutes, the mixture was cooled to room temperature, concentrated in vacuo and chromatographed on silica using 10:90 CH3OH/ethyl acetate as an eluent. The fractions containing the desired product were combined and concentrated to a thick oil, which solidified on refrigeration. This solid (5.3 g) was triturated with hexane three times to provide the product as a white solid, m.p. 77°-79° 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-ee331e0211f14d84a9a360bd9641a669 |
| 出典メモ | uspto-grants-1999_02 |