Sodium Carbonate → HCID 15951413、化合物

HRID 271114ノート

反応式

HRID 271114 の反応式
[C:1]1([C:7](=O)[C:8]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3]C=1.Cl.[CH3:18][NH:19][C:20]([NH2:22])=[NH:21].[C:23]([O-:26])([O-])=O.[Na+].[Na+]>CCO.O>[NH2:22][C:20]1[N:19]([CH3:18])[C:23](=[O:26])[C:8]([C:7]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:1]=2)([C:10]2[CH:11]=[CH:12][N:13]=[CH:14][CH:15]=2)[N:21]=1

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 2750111-Phenyl-2-pyridin-4-ylethane-1,2-dioneHCID 178485118HCID 178485118、化合物

生成物 1

HCID 15951413HCID 15951413、化合物収率 62%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

A suspension of 1-phenyl-2-pyridin-4-ylethane-1,2-dione (0.81 g, 3.8 mmol), N-methylguanidine hydrochloride (1.92 g, 17.5 mmol) and Na2CO3 (3.71 g, 35 mmol) in EtOH (25 mL) and H2O (5 mL) is refluxed for 18 h. The reaction mixture is cooled and poured into water. The precipitate is collected by filtration, washed with water, and air-dried to give the title compound (0.62 g, 62%) as a solid. Mp 154-155° C. MS (+) ES: 267 (M+H)+.

後処理

  1. temperatureis refluxed for 18 h
  2. temperatureThe reaction mixture is cooled
  3. filtrationThe precipitate is collected by filtration
  4. washwashed with water
  5. customair-dried

出典と根拠

ORDレコード
ord-706075c3babf4dd684bd9f7557cabc6a
出典データセット
uspto-grants-2008_11
特許番号
US07452885B2

反応ノート

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