Sodium ethoxide → HCID 178505926、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[C:14]([F:16])[CH:15]=1)[CH2:5][NH:6][C:7](=[S:12])[NH:8][NH:9][CH:10]=O.[O-]CC.[Na+]>>[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[C:14]([F:16])[CH:15]=1)[CH2:5][N:6]1[CH:10]=[N:9][N:8]=[C:7]1[SH:12]参加物
3
実験手順
The crude 4-(3',5'-difluorobenzyl)-1-formyl-3-thiosemicarbazide (3.5 g) was refluxed overnight in a solution of sodium ethoxide (from sodium (0.3 g) in ethanol (25 ml.)). The reaction was filtered, evaporated to dryness, and diluted with water. The aqueous solution was acidified to pH 3-4 with 10% hydrochloric acid, and the precipitate was collected by filtration and recrystallized from ethanol-water to yield 2.3 g (71%) of 4-(3',5'-difluorobenzyl)-1,2,4-triazole-3-thiol after recrystallization from water, m.p.: 129°-130° C.
後処理
- filtrationThe reaction was filtered
- customevaporated to dryness
- additiondiluted with water
- filtrationthe precipitate was collected by filtration
- customrecrystallized from ethanol-water
出典と根拠
- ORDレコード
- ord-2ac4cdb34a904801b0a6be4121fbb0ee
- 出典データセット
- uspto-grants-1986_12
- 特許番号
- US04628059
反応ノート
読み込み中…