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

HRID 8926

反応式

HRID 8926 の反応式
[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

反応物 3

HCID 313Hydrochloric AcidHCID 1048PyrazoleHCID 15112Dimethylcyanamide

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒

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

  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

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

関連ノート

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