Hydrochloric Acid → N,N-dimethyl-1H-pyrazole-1-carboxamidine hydrochloride

HRID 8926

반응식

HRID 8926 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

반응물 3

HCID 313Hydrochloric AcidHCID 1048PyrazoleHCID 15112Dimethylcyanamide

생성물 1

HCID 21984986N,N-dimethyl-1H-pyrazole-1-carboxamidine hydrochloride수율 78%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매

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

  1. temperatureto reflux for 3 hours
  2. customto precipitate a yellow solid
  3. custombottom of the flask (overnight)
  4. customthe supernatant solution was decanted
  5. 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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