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Dimethylcarbamoyl Chloride → 4-[[(Dimethylamino)methylene]amino]-3-pyridinol N,N-dimethylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-[[(Dimethylamino)methylene]amino]-3-pyridinol | HCID 15380929 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 4-[[(Dimethylamino)methylene]amino]-3-pyridinol N,N-dimethylcarbamate | HCID 53834743 | — |
反応手順
4-[[(Dimethylamino)methylene]amino]-3-pyridinol (1.65 g) was refluxed for 1 hour in 20 ml of benzene containing 1.10 g of Et3N and 1.10 g of N,N-dimethylcarbamyl chloride. At the end of this time, the reaction mixture was applied directly to a silica column and eluted with 5% Et3N/ethyl acetate. Concentration of the product-containing fractions gave 2.05 g of chromatographically pure product which was distilled in a bulb to bulb apparatus (oven temperature=175° C.) to give analytically pure material, m.p. 64°-66° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05866565 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-8a762fe76646452cb4ce7d723fce3fb4 |
| 出典メモ | uspto-grants-1999_02 |