Hydrochloric Acid → N,N-dimethyl-1H-pyrazole-1-carboxamidine hydrochloride
反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.[CH3:6][N:7]([CH3:10])[C:8]#[N:9].[ClH:11]>O1CCOCC1.CCOCC>[ClH:11].[CH3:6][N:7]([CH3:10])[C:8]([N:1]1[CH:5]=[CH:4][CH:3]=[N:2]1)=[NH:9]参加物
6
実験手順
To a solution of pyrazole (1.01 g, 14.8 mmol) and dimethylcyanamide (1.20 mL, 14.8 mmol) in 1,4-dioxane (15 mL) was added HCl (4.0 N in 1,4-dioxane, 3.8 mL, 15.2 mmol) and the resultant mixture was heated to reflux for 3 hours. The reaction mixture was cooled to room temperature and diluted with dry ether (15 mL) to precipitate a yellow solid. The resultant precipitate was allowed to settle to the bottom of the flask (overnight) and the supernatant solution was decanted. The solid was dried under vacuum and provided the title compound (2.01 g, 78%). ES-MS m/z 139 (M+H).
後処理
- temperatureto reflux for 3 hours
- customto precipitate a yellow solid
- custombottom of the flask (overnight)
- customthe supernatant solution was decanted
- customThe solid was dried under vacuum
出典と根拠
- ORDレコード
- ord-f311fc80c113400083d5a3966db9b7c5
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091217B2
反応ノート
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