Hydrochloric Acid → 4-Fluoro-1H-pyrazole-1-carboximidamide hydrochloride
反応式
[F:1][C:2]1[CH:3]=[N:4][NH:5][CH:6]=1.[N:7]#[C:8][NH2:9].[ClH:10]>O1CCOCC1>[ClH:10].[F:1][C:2]1[CH:3]=[N:4][N:5]([C:8]([NH2:9])=[NH:7])[CH:6]=1参加物
5
実験手順
To 4-fluoro-1H-pyrazole, 28-d, (2 g, 23 mmol) and cyanamide (0.97 g, 23 mmol) in dioxane (5 mL) was added 4N HCl in dioxane (15 mL). The mixture was gently refluxed with stirring for 2 h under nitrogen. During the course of the reaction the product crystallizes. After cooling to room temperature, 10 mL of anhydrous ether was added and the mixture was allowed to stand for 30 min. The white solid was collected by filtration, washed with anhydrous ether and dried to constant weight in vacuuo providing the product, 28-e, (3 g, 80%).
後処理
- temperatureThe mixture was gently refluxed
- customDuring the course of the reaction the product
- customcrystallizes
- addition10 mL of anhydrous ether was added
- waitto stand for 30 min
- filtrationThe white solid was collected by filtration
- washwashed with anhydrous ether
- customdried to constant weight in vacuuo
出典と根拠
- ORDレコード
- ord-fbef5dc8bcd14603adc0554f21fabe3c
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09079930B2
反応ノート
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