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Aluminum(III) Chloride → HCID 13192925, 화합물

HRID 1579395
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HRID 1579395 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[CH2:5]([O:7][C:8]([C:10]1[CH:25]=[CH:24][C:13]([O:14][C:15]2[N:23]=[CH:22][CH:21]=[CH:20][C:16]=2[C:17](Cl)=[O:18])=[CH:12][CH:11]=1)=[O:9])[CH3:6]>[N+](C1C=CC=CC=1)([O-])=O>[O:18]=[C:17]1[C:16]2[C:15](=[N:23][CH:22]=[CH:21][CH:20]=2)[O:14][C:13]2[CH:12]=[CH:11][C:10]([C:8]([O:7][CH2:5][CH3:6])=[O:9])=[CH:25][C:24]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) Chloride2회HCID 21568403HCID 21568403, 화합물

생성물 1

HCID 13192925HCID 13192925, 화합물수율 56.8%

시약·촉매·용매 1

HCID 7416Nitrobenzene용매

실험 절차

1.7 g of anhydrous aluminum chloride is added in small portions to a solution of 1.2 g of 2-(p-ethoxycarbonylphenoxy)nicotinoyl chloride in 5 ml of nitrobenzene at room temperature with stirring. The mixture is stirred at 80°C for 4 hours, and poured into ice water to decompose aluminum chloride. The nitrobenzene layer is separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue is recrystallized from ethanol to give 0.6 g of ethyl 5-oxo-5H-[1]benzopyrano[2,3-b]pyridine-7-carboxylate melting at 131°-132°C.

후처리

  1. stirringThe mixture is stirred at 80°C for 4 hours
  2. customThe nitrobenzene layer is separated
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-f384b5bc117a499bb2d54793ca660eb4
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03931199

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