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Chloride → 6-Amino-2-methoxy-4-(4-acetoxybutyl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloride | HCID 312 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Butanol, 4-bromo-, 1-acetate | HCID 78491 | — |
| 反応物 | 6-Amino-2-methoxy-3,4-dihydropyrimidin-4-one | HCID 135404214 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 6-Amino-2-methoxy-4-(4-acetoxybutyl)pyrimidine | HCID 23499088 | 42% |
反応手順
Alternative Method B. A mixture of 6-amino-2-methoxy-4-pyrimidone (30 g, 212.6 mmol), K2CO3 (44 g, 318 mmol), benzyltriethylammionium chloride (20 g, 88 mmol) and 4-bromobutyl acetate (60 g, 308 mmol) in acetone (800 ml) was heated at reflux overnight. After cooling to room temperature, the insoluble salts were filtered off and the solvent was removed. The residue was purified by chromatography on silica gel with CHCl3/MeOH (100:2-100:5) as eluent. After separation of 6-amino-2-methoxy-4-(4-acetoxybutyl)pyrimidine (22.8, yield 42%), 18.7 g (yield 34.5%) of 6-amino-2-methoxy-3-(4-acetoxybutyl)-4-pyrimidone was isolated as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06777420B2 |
| 出典データセット | uspto-grants-2004_08 |
| ORD ID | ord-c02c628edb0048c4a13daa4ec2f86a16 |
| 出典メモ | uspto-grants-2004_08 |