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Phosphorus tribromide → 5-(1-Bromoethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | 5-(1-Hydroxyethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine | HCID 20151397 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(1-Bromoethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine | HCID 20151394 | — |
反応手順
A solution of 5-(1-hydroxyethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (1.8 g) in tetrahydrofuran (10 ml) was dropped to a solution of phosphorus tribromide (0.34 ml) in tetrahydrofuran (20 ml) under ice cooling. The reaction mixture was stirred for 5 hours at the same condition and poured into ice water and extracted with ethyl acetate. The organic layer was evaporated in vacuo. The residue was chromatographed on silicagel eluting with chloroform. The fractions containing the desired product were combined and evaporated in vacuo. The residue was crystallized from diisopropyl ether to afford 5-(1-bromoethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (0.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727073 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-d873a469a1aa4c19a659d20fa347bd64 |
| 出典メモ | uspto-grants-1988_02 |