4-Nitrophenol → 1,1'-Oxybis(4-nitrobenzene)

HRID 1595150

반응식

HRID 1595150 반응식
[OH-:1].[K+].[N+:3]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)([O-:5])=[O:4]>C(OCC)(=O)C.CCCCCC>[N+:3]([C:6]1[CH:11]=[CH:10][C:9]([O:12][C:9]2[CH:10]=[CH:11][C:6]([N+:3]([O-:4])=[O:1])=[CH:7][CH:8]=2)=[CH:8][CH:7]=1)([O-:5])=[O:4]

참가 물질

4

반응물 2

HCID 9804-NitrophenolHCID 14797Potassium Hydroxide

생성물 1

HCID 75681,1'-Oxybis(4-nitrobenzene)수율 73.6%

시약·촉매·용매 1

HCID 21226206Ethyl acetate hexane용매2회

실험 절차

Using N-Boc-L-tHyp(Tosyloxy)-OMe (5g, 10.5 mmol), powdered KOH (1.75 g, 26.5 mmol) and 4-nitrophenol (3.66 g, 26.3 mmol) after 4 days at reflux, 2.52 g (65%) of the corresponding 4-nitrophenyl ether was obtained by column chromatography (silica ge, ethyl acetate/hexane mixtures) and crystallization of the appropriate fractions from ethyl acetate/hexane (1:1). An alternate method is to triturate the oily crude and pentane several times [hexane doesn't work] and then add a very, small amount of ethyl acetate to solidify the product. The filtered, solid product may than be crystallized as above. Elemental analysis for C17H22N2O7 (366.324 g/mmol): Calculated C, 55.74; H, 6.05; N, 7.65. Found C, 55.71; H, 6.05; N, 7.65.

후처리

  1. customafter 4 days
  2. temperatureat reflux

출처 및 근거

ORD 기록
ord-582a682f9f7e4b44b28e4c4b59f13b65
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06288036B1

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