Potassium Carbonate → (5-Chlorothiophen-3-yl)methanamine hydrochloride
反応式
[Cl:1]N1C(=O)CCC1=O.[S:9]1[CH:13]=[CH:12][C:11]([C:14]#[N:15])=[CH:10]1.C([O-])([O-])=O.[K+].[K+]>CCCCCC>[ClH:1].[Cl:1][C:13]1[S:9][CH:10]=[C:11]([CH2:14][NH2:15])[CH:12]=1参加物
5
実験手順
To a solution of N-chlorosuccinimide (1.0 eq, 12.2 g) in hexane (100 mL) were added thiophene-3-carbonitrile (10 g, 91.6 mmol) and 70% HClO4 (1 mol %, 0.1 mL). The reaction mixture was stirred overnight at room temperature and subsequently K2CO3 was added. Removal of the solids and the volatiles afforded the crude product as a yellow oil. (This was a mixture of starting material: desired product: wrong isomer: dichlorinated 48%:26%:19%:6%.) Purification twice by column chromatography afforded 5-chlorothiophene-3-carbonitrile (1.71 g, 13%) as a yellow oil.
後処理
- customRemoval of the solids
- customthe volatiles afforded the crude product as a yellow oil
- additiona mixture of starting material
出典と根拠
- ORDレコード
- ord-7565e5a9a84e4f958682b62a8fb6e441
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08148380B2
反応ノート
読み込み中…