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Potassium Carbonate → 2-{3-[3-(Dibenzothiophen-4-yl)phenyl]phenyl}dibenzo[f,h]quinoline

HRID 626606
ノート
印刷プレビュー

反応式

HRID 626606 の反応式
Br[C:2]1[CH:3]=[C:4]([C:8]2[CH:17]=[CH:16][C:15]3[C:10](=[C:11]4[CH:25]=[CH:24][CH:23]=[CH:22][C:12]4=[C:13]4[CH:21]=[CH:20][CH:19]=[CH:18][C:14]4=3)[N:9]=2)[CH:5]=[CH:6][CH:7]=1.[CH:26]1[C:34]2[C:33]3[CH:35]=[CH:36][CH:37]=[CH:38][C:32]=3[S:31][C:30]=2[C:29]([C:39]2[CH:40]=[C:41](B(O)O)[CH:42]=[CH:43][CH:44]=2)=[CH:28][CH:27]=1.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.C(=O)([O-])[O-].[K+].[K+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CO.C1(C)C=CC=CC=1.O.C(O)C>[CH:26]1[C:34]2[C:33]3[CH:35]=[CH:36][CH:37]=[CH:38][C:32]=3[S:31][C:30]=2[C:29]([C:39]2[CH:40]=[C:41]([C:2]3[CH:3]=[C:4]([C:8]4[CH:17]=[CH:16][C:15]5[C:10](=[C:11]6[CH:25]=[CH:24][CH:23]=[CH:22][C:12]6=[C:13]6[CH:21]=[CH:20][CH:19]=[CH:18][C:14]6=5)[N:9]=4)[CH:5]=[CH:6][CH:7]=3)[CH:42]=[CH:43][CH:44]=2)=[CH:28][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 11430Potassium CarbonateHCID 80271Tri-o-tolylphosphineHCID 58261920(3-(Dibenzo[b,d]thiophen-4-yl)phenyl)boronic acidHCID 866755632-(3-Bromophenyl)dibenzo[f,h]quinoline

生成物 1

HCID 866755622-{3-[3-(Dibenzothiophen-4-yl)phenyl]phenyl}dibenzo[f,h]quinoline収率 63%

試薬・触媒・溶媒 5

HCID 167845
palladium(II) acetate
触媒
HCID 702Ethanol溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒2 回

実験手順

In a 50-mL three-neck flask, 0.56 g (1.5 mmol) of 2-(3-bromophenyl)dibenzo[f,h]quinoline, 0.46 g (1.5 mmol) of 3-(dibenzothiophen-4-yl)phenylboronic acid, 58 mg (0.19 mmol) of tri(ortho-tolyl)phosphine, 15 mL of toluene, 1.5 mL of ethanol, and 1.5 mL of a 2M aqueous solution of potassium carbonate were put. The mixture was degassed by being stirred under reduced pressure, and the air in the flask was replaced with nitrogen. Then, 17 mg (77 μmol) of palladium(II) acetate was added to this mixture, and the mixture was stirred at 80° C. for 9 hours under a nitrogen stream. After a predetermined time, water and toluene were added to this mixture, and the resulting solid was collected by suction filtration. A toluene solution of the obtained solid was suction-filtered through alumina and Celite, and the filtrate was concentrated to give a yellow solid. A methanol suspension of the obtained solid was irradiated with ultrasonic waves, and a solid was collected by suction filtration, so that the object of the synthesis was obtained as 0.52 g of white powder in 63% yield.

後処理

  1. customThe mixture was degassed
  2. stirringthe mixture was stirred at 80° C. for 9 hours under a nitrogen stream
  3. filtrationthe resulting solid was collected by suction filtration
  4. filtrationA toluene solution of the obtained solid was suction-filtered through alumina and Celite
  5. concentrationthe filtrate was concentrated
  6. customto give a yellow solid
  7. customwas irradiated with ultrasonic waves
  8. filtrationa solid was collected by suction filtration, so that the object of the synthesis

出典と根拠

ORDレコード
ord-f9033963dc924b349ea16896d18172f4
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309223B2

反応ノート

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