Hydrochloric Acid → N,N-dimethyl-1H-pyrazole-1-carboxamidine hydrochloride
반응식
[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]참가 물질
6
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f311fc80c113400083d5a3966db9b7c5
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091217B2
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