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Hydrochloric Acid → 5-[(4-Amino-3-methoxyphenyl)methyl]pyrimidine-2,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Methoxyaniline | HCID 7000 | — |
| 反応物 | 2,4-Diamino-5-pyrimidinemethanol | HCID 295878 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-[(4-Amino-3-methoxyphenyl)methyl]pyrimidine-2,4-diamine | HCID 13043128 | 70.8% |
反応手順
A solution of 6.30 g (0.045 mol) of 2,4-diamino-5-hydroxymethylpyrimidine, 6.15 g (0.05 mol) of o-anisidine and 3.75 ml of concentrated hydrochloric acid in 55 ml of glacial acetic acid was heated to reflux for 6 hours. The mixture was stirred at room temperature overnight. The solvent was removed under vaccum and the residue was taken up in water, made basic with ammonium hydroxide, and the aqueous solution was extracted with dichloromethane:methanol/3:1. The organic layers were combined, dried and concentrated to a purple glass. This was purified on a silica gel column to give 7.81 g of the 4-N-acetylated product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04587341 |
| 出典データセット | uspto-grants-1986_05 |
| ORD ID | ord-9654bf1c191345a1808a8d4d149be06c |
| 出典メモ | uspto-grants-1986_05 |