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Carbazole → 1,3-Bis(N-carbazolyl)benzene

HRID 590005
ノート
印刷プレビュー

反応式

HRID 590005 の反応式
CC1(P(C(C)(C)C)C(C)(C)C)[C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)([C:5]2[CH:10]=[CH:9][CH:8]=[CH:7]C=2)C1.[CH:26]1[C:38]2[NH:37][C:36]3[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=3)[C:30]=2[CH:29]=[CH:28][CH:27]=1.C[Mg]Cl.Cl[C:43]1[CH:48]=[CH:47][CH:46]=[C:45](Cl)[CH:44]=1.[Cl-].[NH4+:51]>C1(C)C=CC=CC=1.O.C1COCC1>[CH:35]1[C:36]2[N:37]([C:43]3[CH:48]=[CH:47][CH:46]=[C:45]([N:51]4[C:5]5[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=5[C:11]5[C:12]4=[CH:13][CH:14]=[CH:15][CH:16]=5)[CH:44]=3)[C:38]3[C:30](=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:31]=2[CH:32]=[CH:33][CH:34]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 6854CarbazoleHCID 109431,3-DichlorobenzeneHCID 25517Ammonium ChlorideHCID 21909131Di-tert-butyl(1-methyl-2,2-diphenylcyclopropyl)phosphaneHCID 178418332HCID 178418332、化合物

生成物 1

HCID 220203771,3-Bis(N-carbazolyl)benzene

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 1140Toluene溶媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
5 °C

実験手順

[PdCl(π-allyl)]2 (11.6 mg, 0.1 mol %) and cBRIDP (44.4 mg, 0.4 mol %) were placed into a 50 mL, two-necked, round bottomed flask equipped a gas inlet, and the flask was evacuated and filled with nitrogen. Subsequently, to the mixture was added dehydrated THF (8.2 mL, 101.0 mmol, 3.2 equivalents) to prepare a catalyst solution. A 200 mL, four-necked, round-bottomed flask equipped with a Teflon® coated magnetic stirring bar, condenser, dropping funnel, thermometer, and a gas inlet was evacuated and filled with nitrogen. Carbazole (10.9 g, 65.0 mmol, 2.06 equivalents) and dehydrated xylenes (66 mL) were charged into the flask, and the mixture was cooled to 5° C. using an ice bath. Subsequently, to the mixture was added a THF solution of MeMgCl (3.22 mol/L, 20.0 mL, 64.4 mmol, 2.04 equivalents) dropwise via the dropping funnel at such a rate that the temperature of the reaction solution was kept at 20° C. or lower, and then the dropping funnel was washed with dehydrated xylenes (11 mL). Subsequently, to the solution were added 1,3-dichlorobenzene (3.6 mL, 31.6 mmol, 1.0 equivalent) and the catalyst solution (8.2 mL) successively, and the solution was stirred for 10 minutes under reflux. After cooling the reaction mixture to room temperature, to the mixture were added water (25 mL) and ammonium chloride (1.7 g). The aqueous layer was separated off, and the organic layer was concentrated under reduced pressure to give solid residue. The residue was dissolved in toluene, and the solution was decolorized by silica gel (1 g) and filtered through a Celite pad. The filtrate was concentrated under reduced pressure to give the solid, which was recrystallized from toluene/methanol to afford 12.5 g of mCP as a white powder.

後処理

  1. customtwo-necked, round bottomed flask equipped a gas inlet
  2. customthe flask was evacuated
  3. additionfilled with nitrogen
  4. customto prepare a catalyst solution
  5. customthermometer, and a gas inlet was evacuated
  6. additionfilled with nitrogen
  7. customwas kept at 20° C.
  8. washlower, and then the dropping funnel was washed with dehydrated xylenes (11 mL)
  9. temperatureunder reflux
  10. temperatureAfter cooling the reaction mixture to room temperature
  11. customThe aqueous layer was separated off
  12. concentrationthe organic layer was concentrated under reduced pressure
  13. customto give solid residue
  14. filtrationfiltered through a Celite pad
  15. concentrationThe filtrate was concentrated under reduced pressure
  16. customto give the solid, which
  17. customwas recrystallized from toluene/methanol
  18. customto afford 12.5 g of mCP as a white powder

出典と根拠

ORDレコード
ord-99238480d0104be9bee307d3ffb0ae57
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09233922B2

反応ノート

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