Sodium Iodide → HCID 22707973, 화합물

HRID 353214노트

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HRID 353214 반응식
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[NH:11][C:10](=[O:12])[C:9]([C:13]#[N:14])=[CH:8][CH:7]=1.Cl[CH2:16][C:17]([NH2:19])=[O:18].[I-].[Na+].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.C(OCC)(=O)C.O>[C:13]([C:9]1[C:10]([O:12][CH2:16][C:17]([NH2:19])=[O:18])=[N:11][C:6]([C:2]2[O:1][CH:5]=[CH:4][CH:3]=2)=[CH:7][CH:8]=1)#[N:14]

참가 물질

8

반응물 4

HCID 5238Sodium IodideHCID 6580ChloroacetamideHCID 11430Potassium CarbonateHCID 27470886-(Furan-2-yl)-2-oxo-1,2-dihydropyridine-3-carbonitrile

생성물 1

HCID 22707973HCID 22707973, 화합물수율 54%

시약·촉매·용매 3

HCID 180Acetone용매HCID 962Water용매HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

A suspension of 6-(2-furyl)-2-oxo-1,2-dihydro-3-pyridinecarbonitrile (6.0 g, 32.3 mmol), 2-chloroacetamide (3.0 g, 37.7 mmol), sodium iodide (5.7 g, 38.0 mmol) and potassium carbonate (9.0 g, 56.2 mmol) in acetone (100 ml) was stirred at 60° C. for 6 hours. After cooling as it was, the reaction solution was diluted with ethyl acetate and water. The organic layer was washed with an aqueous saturated solution of sodium bicarbonate (×2) and an aqueous saturated solution of ammonium chloride, dried over anhydrous sodium sulfate, and concentrated. Diethyl ether was added to the residue, and the resulting precipitates were collected by filtration and washed with diethyl ether, to give the title compound (4.2 g, 54%) as a brown solid.

후처리

  1. temperatureAfter cooling as it
  2. washThe organic layer was washed with an aqueous saturated solution of sodium bicarbonate (×2)
  3. dry with materialan aqueous saturated solution of ammonium chloride, dried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. additionDiethyl ether was added to the residue
  6. customthe resulting precipitates
  7. filtrationwere collected by filtration
  8. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-569a59fcda26478c847ca0dbbecc57a7
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06750232B2

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