Sodium Carbonate → HCID 15951413, 화합물

HRID 271114노트

반응식

HRID 271114 반응식
[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

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 2750111-Phenyl-2-pyridin-4-ylethane-1,2-dioneHCID 178485118HCID 178485118, 화합물

생성물 1

HCID 15951413HCID 15951413, 화합물수율 62%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-706075c3babf4dd684bd9f7557cabc6a
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452885B2

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