関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzaldehyde | HCID 240 | — |
| 反応物 | 1,3,4-Thiadiazole, 2-amino-5-methyl- | HCID 66949 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-benzyl-5-methyl-1,3,4-thiadiazol-2-amine | HCID 6460923 | 75.4% |
反応手順
2-Amino-5-methyl-1,3,4-thiadiazole (23 g, 0.2 mole) and benzaldehyde (29.6 ml, 0.3 mole) were refluxed together in ethanol (200 ml) for 11/2 hours. The solution was cooled to room temperature and sodium borohydride (11.35 g, 0.3 mole) added over 5 to 10 minutes. The mixture was refluxed for 4 hours, treated with further sodium borohydride (5 g) and refluxed overnight. The ethanol was evaporated off, the residue treated with water and extracted with ether. The ether extract was dried over sodium sulphate, filtered and evaporated to leave an oil which solidified. This solid was triturated with ether, filtered, washed with light petroleum (b.p. 40°-60° C.) and again triturated with ether and filtered to give N-(5-methyl-1,3,4-thiadiazol-2-yl)-benzylamine (30.95 g), which on recrystallisation from ether had m.p. 140° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04158659 |
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| 出典データセット | uspto-grants-1979_06 |
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| ORD ID | ord-210fbb6c76274aa48c907f4f97d0d15f |
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| 出典メモ | uspto-grants-1979_06 |
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