Sodium → Sodium
反応式
[Na:1].ClC1C(F)=C(F)N=C(F)C=1F.[F:13][C:14]1[C:19]([F:20])=[C:18]([SH:21])[C:17]([F:22])=[C:16]([F:23])[N:15]=1.O.O.[SH-].[Na+]>C(O)(C)C>[F:13][C:14]1[C:19]([F:20])=[C:18]([SH:21])[C:17]([F:22])=[C:16]([F:23])[N:15]=1.[Na:1]参加物
6
実験手順
Preparation of the sodium salt of 2,3,5,6-tetrafluoropyridine-4-thiol 4-Chloro-2,3,5,6-tetrafluoropyridine (2 g) and sodium hydrosulfide dihydrate were stirred and heated under reflux in iso-propanol (40 cm3) for 3 hours. The mixture was then stirred at the ambient temperature for 18 hours. The precipitated solid was removed by filtration, washed with diethyl ether and discarded. The combined organic solutions were evaporated under reduced pressure to give 2,3,5,6-tetrafluoropyridine-4-thiol as its sodium salt (2.21 g), which was used without further purification in the second step.
後処理
- temperatureheated
- stirringThe mixture was then stirred at the ambient temperature for 18 hours
- customThe precipitated solid was removed by filtration
- washwashed with diethyl ether
- customThe combined organic solutions were evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-f97166810e6c4417acdf11c23dd54461
- 出典データセット
- uspto-grants-1999_06
- 特許番号
- US05912243
反応ノート
読み込み中…