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Pyridine → 2-Bromo-4-propionamidothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 2-Bromo-1,3-thiazol-4-amine--hydrogen bromide (1/1) | HCID 20294041 | — |
| 溶媒 | Propionic anhydride | HCID 31263 | — |
| 生成物 | 2-Bromo-4-propionamidothiazole | HCID 20294046 | 11.9% |
反応手順
4-Amino-2-bromothiazole hydrobromide (6.5g.) was suspended in propionic anhydride (25 ml.) with stirring; then treated with pyridine (12.5 ml.) over 15 minutes, maintaining reaction temperature at 0° C. with an ice bath. After the addition was complete, the reaction mixture was stirred for 2 hours at room temperature, then poured onto 20% aqueous sodium acetate (250 ml.) and stirred for 30 minutes. The precipitate was removed by filtration and washed with water. The solid was air dried and extracted with hexane, in a Sexhlet apparatus. The hexane was cooled and the crystals collected and recrystallised to give the title compound (2.8 g.) m.p. 122°-5° C. (Found: C, 31.1; H, 3.1; N, 11.9. C6H7BrN2OS requires C, 30.7; H, 3.0; N, 11.9%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04183854 |
| 出典データセット | uspto-grants-1980_01 |
| ORD ID | ord-7ac404c4c91f435ea6768c7af9ada4d4 |
| 出典メモ | uspto-grants-1980_01 |