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O-Xylene → 3-(1,3,4-Thiadiazol-2-yl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Xylene | HCID 7237 | — |
| 反応物 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 反応物 | 2-(Pyridin-3-yl)-1,3,4-oxadiazole | HCID 4023165 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(1,3,4-Thiadiazol-2-yl)pyridine | HCID 19871284 | — |
反応手順
A mixture of 5.5 g of the above prepared 2-(3-pyridyl)-1,3,4-oxadiazole, 8.5 g of phosphorus pentasulfide and 70 ml of xylene is stirred for 16 hours at 150°-160° C. To the cooled reaction mixture are added 50 ml of water and stirring is continued for another 5 minutes. The reaction mixture is then filtered. The filter residue is taken up in 100 ml of 10% sodium hydroxide solution. After extraction with chloroform, the organic phase is washed with water, dried and concentrated. After purification by column chromatography over silica gel with a 95:5 mixture of chloroform/ethanol as eluant, the crude 2-(3-pyridyl)-1,3,4-thiadiazole (compound 1) of the formula ##STR8## with a melting point of 64°-67° C., is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04892880 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-a2c580c2c4c74133a7367a1650251ce9 |
| 出典メモ | uspto-grants-1990_01 |