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Ammonia → 6-Aminomethyl-4-ethoxy-N-methylnicotinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl methanesulfonate | HCID 57791315 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6-Aminomethyl-4-ethoxy-N-methylnicotinamide | HCID 57791297 | — |
反応手順
4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl methanesulfonate (436 mg), dissolved in abs. MeOH (7 ml), was added dropwise to a methanolic ammonia solution (7.1 ml; 7N) in a microwave vessel at RT and with stirring in the course of 10 min. After standing overnight, the solvent was stripped off and the residue was purified by means of preparative HPLC. The product-containing fractions were combined, freed from the acetonitrile and freeze-dried. The product was treated with saturated sodium chloride solution and rendered alkaline with potassium carbonate. After extraction with methylene chloride, the combined organic phases were dried with sodium sulfate, filtered and concentrated. 71 mg of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863269B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-a36aaf2c062e4b11ab9cb33213235253 |
| 出典メモ | uspto-grants-2011_01 |