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Sodium Iodide → 1-Benzoyloxymethyl-5-bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidinium iodide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Chloromethyl benzoate | HCID 79257 | — |
| 反応物 | 5-Bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidine | HCID 53739887 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Benzoyloxymethyl-5-bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidinium iodide | HCID 67599459 | — |
反応手順
0.3 g (8.2 mmol) of 5-bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidine (according to EP-A-57 440), 0.17 g (9.8 mmol) of chloromethyl benzoate and 0.12 g (8.2 mmol) of sodium iodide in 25 ml of acetone were heated under reflux for 8 hours. After cooling, the precipitated sodium chloride was filtered off and the filtrate was concentrated. The residue was taken up in dichloromethane and washed by stirring with water. The organic phase was dried and concentrated. The residue was digested with ethyl acetate. Filtration with suction gave 0.97 g (53.3% of theory) of light-yellow crystals. mp.: 159-161° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05925644 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-f8a076c500ce4ebcb8ed728ba249b303 |
| 出典メモ | uspto-grants-1999_07 |