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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → Diethyl 2,6-diisopropyl-4-(4-fluorophenyl)-pyridine-3,5-dicarboxylate

HRID 324789
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HRID 324789 반응식
ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl.[CH:15]([C:18]1[NH:19][C:20]([CH:41]([CH3:43])[CH3:42])=[C:21]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[CH:22]([C:29]2[CH:34]=[CH:33][C:32]([F:35])=[CH:31][CH:30]=2)[C:23]=1[C:24]([O:26][CH2:27][CH3:28])=[O:25])([CH3:17])[CH3:16]>ClCCl>[CH:41]([C:20]1[C:21]([C:36]([O:38][CH2:39][CH3:40])=[O:37])=[C:22]([C:29]2[CH:30]=[CH:31][C:32]([F:35])=[CH:33][CH:34]=2)[C:23]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:18]([CH:15]([CH3:17])[CH3:16])[N:19]=1)([CH3:43])[CH3:42]
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참가 물질

4

반응물 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 11661355Diethyl 1,4-dihydro-2,6-diisopropyl-4-(4-fluorophenyl)pyridine-3,5-dicarboxylate

생성물 1

HCID 10179180Diethyl 2,6-diisopropyl-4-(4-fluorophenyl)-pyridine-3,5-dicarboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

171.7 g (0.757 mol) of 2,3-dichloro-5,6-dicyano-p-benzoquinone is added to a solution of 304.8 g (0.757 mol) of the compound from Example VII in 2 l of dichloromethane, and the mixture is stirred overnight at room temperature. The mixture is drawn off by suction over diatomaceous earth and subsequently washed well with dichloromethane. After concentration of the dichloromethane phase to a volume of approx. 800 ml, it is chromatographed on a column (2 kg of silica gel 70-230 mesh) with dichloromethane.

후처리

  1. washsubsequently washed well with dichloromethane
  2. customAfter concentration of the dichloromethane phase to a volume of approx. 800 ml, it is chromatographed on a column (2 kg of silica gel 70-230 mesh) with dichloromethane

출처 및 근거

ORD 기록
ord-a9208d18621d4418b20b8fadd3df1c50
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218431B1

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