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Dimethylcarbamoyl Chloride → 4-[[(1-Piperidinyl)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-[[(1-Piperidinyl)methylene]amino]-3-pyridinol | HCID 15380933 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-[[(1-Piperidinyl)methylene]amino]-3-pyridinol N,N-dimethylcarbamate | HCID 67749070 | — |
反応手順
A mixture prepared from 4-[[(1-piperidinyl)methylene]amino]-3-pyridinol (3.5 g), triethylamine (3.69 mL), dimethylcarbamyl chloride (2.3 mL) and tetrahydrofuran (130 mL) was refluxed for 2 hours, filtered, poured directly onto a silica column and eluted successively with ethyl acetate and 5% Et3N/ethyl acetate to yield 4.49 g of product. Recrystallization from ethyl acetate and drying under high vacuum yielded 3.94 g of crystals, m.p. 88°-89° 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-5ed5ad72f5c241399727961c6ecec419 |
| 出典メモ | uspto-grants-1999_02 |