Potassium Carbonate → 4-(2-Propynylthio)pyridine
反応式
[SH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:14](Cl)[C:15]#[CH:16]>CS(C)=O>[CH2:16]([S:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1)[C:15]#[CH:14]参加物
5
反応条件
- 温度
- 60 °C
実験手順
In 200 ml dimethyl sulfoxide (DMSO) was dissolved 25.0 g (0.225 mole) 4-mercaptopyridine. To this solution were added 15.5 g (0.112 mole) anhydrous potassium carbonate and 16.5 g (0.25 mole) propargyl chloride. This mixture was heated at 60° C. for 3 hours. The reaction mixture was then cooled to room temperature and filtered. The filtrate was added to an equal volume of water. This mixture was extracted with ether. After removal of the ether under reduced pressure, there remained 20.0 g crude product. Distillation gave 13.5 g 4-(2-propynylthio)pyridine. Yield 39% theory; b.p. 79°-81° C. (1.0 mm); mp 55°-56° C.
後処理
- temperatureThe reaction mixture was then cooled to room temperature
- filtrationfiltered
- additionThe filtrate was added to an equal volume of water
- extractionThis mixture was extracted with ether
- customAfter removal of the ether under reduced pressure, there
- distillationDistillation
出典と根拠
- ORDレコード
- ord-75984f85d1ae4df1a43913435b44f7c4
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04220577
反応ノート
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