Potassium Carbonate → HCID 59306790, 화합물

HRID 1052922노트

반응식

HRID 1052922 반응식
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

참가 물질

7

반응물 3

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

생성물 1

HCID 59306790HCID 59306790, 화합물수율 156.6%

시약·촉매·용매 3

HCID 80271Tri-o-tolylphosphine촉매HCID 167845palladium(II) acetate촉매HCID 80711,2-Dimethoxyethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aedd0a95f7814e328937bb8ee0dd8f88
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09391288B2

반응 노트

불러오는 중…