Potassium Carbonate → HCID 59306790、化合物

HRID 1052922ノート

反応式

HRID 1052922 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]2[NH:6][C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3.[C:15]1([N:21]2[C:33]3C=C(B4OC(C)(C)C(C)(C)O4)C=C[C:28]=3[C:27]3[C:22]2=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.COCCOC>[C:15]1([N:21]2[C:22]3[CH:23]=[C:24]([C:2]4[CH:3]=[CH:4][C:5]5[NH:6][C:7]6[C:12]([C:13]=5[CH:14]=4)=[CH:11][CH:10]=[CH:9][CH:8]=6)[CH:25]=[CH:26][C:27]=3[C:28]3[C:33]2=[CH:3][CH:2]=[CH:14][CH:13]=3)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 2524463-BromocarbazoleHCID 598587389- Phenyl-2-(4,4,5,5-tetraMethyl- 1,3,2-dioxaborolan-2-yl)-9H-carbazole

生成物 1

HCID 59306790HCID 59306790、化合物収率 156.6%

試薬・触媒・溶媒 3

HCID 80271Tri-o-tolylphosphine触媒HCID 167845palladium(II) acetate触媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

Next, a mixed solution of 4.0 g of 3-bromocarbazole, 6.6 g of 9-phenyl-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolane-2-yl)-9H-carbazole, 18 ml of a 2M aqueous potassium carbonate solution, 80 ml of 1,2-dimethoxyethane, 72 mg of palladium acetate and 243 mg of tris(2-methylphenyl)phosphine was refluxed for 6 hours under a nitrogen flow. The solution was cooled to room temperature, and then extracted with toluene. The organic layer was washed with water twice, dried over magnesium sulfate, and then evaporated. The resultant concentrate was purified by silica gel column chromatography and then vacuum-dried to obtain 5.2 g of 9-phenyl-9H,9′H-2,3′-bicarbazole.

後処理

  1. extractionextracted with toluene
  2. washThe organic layer was washed with water twice
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. concentrationThe resultant concentrate
  6. customwas purified by silica gel column chromatography
  7. customvacuum-dried

出典と根拠

ORDレコード
ord-aedd0a95f7814e328937bb8ee0dd8f88
出典データセット
uspto-grants-2016_07
特許番号
US09391288B2

反応ノート

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