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Diisopropylethylamine → 4-[3-(1-t-Butoxycarbonylpiperidin-4-yl)propenoyl]nitrobenzene

HRID 976141
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인쇄 미리보기

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HRID 976141 반응식
[Cl-].[Li+].C(N(C(C)C)CC)(C)C.[CH:12]([CH:14]1[CH2:19][CH2:18][N:17]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:16][CH2:15]1)=O.[N+:27]([C:30]1[CH:46]=[CH:45][C:33]([C:34]([CH2:36]P(=O)(OCC)OCC)=[O:35])=[CH:32][CH:31]=1)([O-:29])=[O:28]>C(#N)C.O>[C:23]([O:22][C:20]([N:17]1[CH2:18][CH2:19][CH:14]([CH:12]=[CH:36][C:34]([C:33]2[CH:32]=[CH:31][C:30]([N+:27]([O-:29])=[O:28])=[CH:46][CH:45]=2)=[O:35])[CH2:15][CH2:16]1)=[O:21])([CH3:26])([CH3:25])[CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 433294Lithium ChlorideHCID 1514430tert-Butyl 4-formylpiperidine-1-carboxylateHCID 11808775Diethyl [2-(4-nitrophenyl)-2-oxoethyl]phosphonate

생성물 1

HCID 569933314-[3-(1-t-Butoxycarbonylpiperidin-4-yl)propenoyl]nitrobenzene수율 73.6%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6342Acetonitrile용매

실험 절차

0.28 g of lithium chloride, 0.85 g of diisopropylethylamine and 2.13 g of 4-formyl-l-t-butoxycarbonylpiperidine were added to 2.0 g of diethyl (4-nitrobenzoylmethyl)phosphonate dissolved in 20 ml of acetonitrile, and the mixture was stirred at room temperature for about 3 days. Then, water was added to the reaction mixture, and the mixture was extracted with toluene. The extract was dried over anhydrous sodium sulfate and condensed. The obtained residue was applied to silica gel column chromatography to obtain 1.76 g of the title compound as pale yellow crystal.

후처리

  1. extractionthe mixture was extracted with toluene
  2. dry with materialThe extract was dried over anhydrous sodium sulfate and condensed

출처 및 근거

ORD 기록
ord-9f7d2904910a4743b4b55aecdf81432b
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05610303

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