化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 5-[(5-Chloro-2,6-dimethylpyrimidin-4-ylamino)methyl]-2-methoxyphenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | (3-Benzyloxy-4-methoxybenzyl)(5-chloro-2,6-dimethylpyrimidin-4-yl)amine | HCID 22639999 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-[(5-Chloro-2,6-dimethylpyrimidin-4-ylamino)methyl]-2-methoxyphenol | HCID 22640027 | 81.2% |
反応手順
In analogy to the method described in example B1, 3.0 g (7.8 mmol) of (3-benzyloxy-4-methoxy-benzyl)(5-chloro-2,6-dimethylpyrimidin-4-yl)amine (from example A4) are reacted with 30 ml of 12.5N hydrochloric acid in 30 ml of ethanol. Extraction with ethyl acetate at a pH of 8 gives, after concentration, a solid residue which is chromatographed on silica gel (mobile phase: toluene/dioxane=5:1). Crystallization from toluene/methanol gives 1.86 g (72%) of the title compound as a beige crystallizate. m.p.: 165-168° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06818642B2 |
| 出典データセット | uspto-grants-2004_11 |
| ORD ID | ord-06d98458d60647c4a9c22b5e250ddeec |
| 出典メモ | uspto-grants-2004_11 |