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Water → 5,6-Bis(4-bromophenyl)-2,2'-bipyridine

HRID 1502563
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HRID 1502563 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=3)N=N[C:13]=2[C:14]2[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][CH:15]=2)=[CH:4][CH:3]=1.[CH:27]12CC(C=C1)C=[CH:28]2.C1(C)C(C)=CC=CC=1.O>C1(C)C=CC=CC=1>[Br:20][C:17]1[CH:18]=[CH:19][C:14]([C:13]2[CH:27]=[CH:28][C:10]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=3)=[N:9][C:8]=2[C:5]2[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][CH:4]=2)=[CH:15][CH:16]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 7237O-XyleneHCID 8473NorbornadieneHCID 579585455,6-Bis(4-bromophenyl)-3-(2-pyridyl)-1,2,4-triazine

생성물 1

HCID 579585085,6-Bis(4-bromophenyl)-2,2'-bipyridine수율 59.6%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
140 °C

실험 절차

In a 500 mL three-neck flask were put 13 g (27 mmol) of 5,6-bis(4-bromophenyl)-3-(2-pyridyl)-1,2,4-triazine, 9.0 mL (83 mmol) of 2,5-Norbornadiene, and 150 mL of xylene. This mixture was refluxed at 140° C. for 5 hours under a nitrogen stream. After a certain time, water was added to the mixture, and an aqueous layer was extracted with toluene. The extract was washed with a saturated saline together with the organic layer, and the organic layer was then dried with magnesium sulfate. The mixture was subjected to gravity filtration, and the obtained filtrate was concentrated to give a solid. The solid was refined with silica gel column chromatography (toluene), so that a target substance, 7.5 g of light-yellow powder was obtained in a yield of 59%.

후처리

  1. customIn a 500 mL three-neck flask were put
  2. extractionan aqueous layer was extracted with toluene
  3. washThe extract was washed with a saturated saline together with the organic layer
  4. dry with materialthe organic layer was then dried with magnesium sulfate
  5. filtrationThe mixture was subjected to gravity filtration
  6. concentrationthe obtained filtrate was concentrated
  7. customto give a solid

출처 및 근거

ORD 기록
ord-b62f033a0c094bbeaaf3c9f1834392e0
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09209408B2

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