1,4-Dioxane → Ethyl 2-nitro-3-(3-nitrophenyl)-5-oxo-5-phenylpentanoate

HRID 2106807

반응식

HRID 2106807 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:13])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[N+:20]([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])([O-:22])=[O:21].O1CCOCC1>N1CCCCC1.C(O)C>[N+:20]([CH:23]([CH:10]([C:6]1[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=1)[CH2:11][C:12](=[O:13])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:24]([O:26][CH2:27][CH3:28])=[O:25])([O-:22])=[O:21]

참가 물질

6

반응물 3

HCID 312751,4-DioxaneHCID 69379Ethyl nitroacetateHCID 948623-Nitrochalcone

생성물 1

HCID 10068705Ethyl 2-nitro-3-(3-nitrophenyl)-5-oxo-5-phenylpentanoate수율 19.7%

시약·촉매·용매 2

HCID 8082Piperidine촉매HCID 702Ethanol용매

실험 절차

A mixture of 3-(3-nitrophenyl)-1-phenyl-2-propen-1-one (0.5 g), ethyl nitroacetate (0.29 g), piperidine (3 drops), dioxane (5 ml) and ethanol (5 ml) was refluxed for 2 hours. After allowing to cooling at ambient temperature, the reaction mixture was evaporated in vacuo. The residue was subjected to a column chromatography on silica gel (50 ml) eluting with benzene. The fractions containing the object compound were combined and concentrated under reduced pressure to give ethyl 2-nitro-3-(3-nitrophenyl)-5-oxo-5-phenylpentanoate (0.15 g).

후처리

  1. temperaturewas refluxed for 2 hours
  2. customthe reaction mixture was evaporated in vacuo
  3. washeluting with benzene
  4. additionThe fractions containing the object compound
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-49572627f23b4d279249946b81bcf962
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04931453

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