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2-Aminothiophenol → 2-(5-Methylpyridin-2-yl)-1,3-benzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Aminothiophenol | HCID 8713 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 5-Methylpicolinic acid | HCID 199575 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(5-Methylpyridin-2-yl)-1,3-benzothiazole | HCID 12354112 | 88.4% |
反応手順
22.5 g (0.18 mol) of o-aminothiophenol, 25 g (0.18 mol) of 5-methylpicolic acid and 100 g of polyphosphoric acid were admixed and stirred in nitrogen gas streams at 170°-200° C. and the mixture was poured in 1 l of water. The mixture was adjusted to pH 5 with an aqueous solution of sodium hydroxide and the resulting crystals were recovered by filtration, whereupon 40 g of 2-(benzothiazol-2-yl)-5methylpyridine was obtained as crude crystals. This crude product was recrystallized from ligroine. By the above procedure was obtained 36 g of the same compound as colorless flakes melting at 169.5°-170.0° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04232010 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-a78161e6770442f0bac33bd238d93fb8 |
| 出典メモ | uspto-grants-1980_11 |