Triphenylsilane → HCID 86676047, 화합물

HRID 1502195노트

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HRID 1502195 반응식
[C:1]([N:4]1[C:16]2[CH:15]=[CH:14][C:13](I)=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[C:8](I)[CH:9]=2)(=[O:3])[CH3:2].[C:19]1([SiH:25]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>CN1CCCC1=O>[C:1]([N:4]1[C:16]2[CH:15]=[CH:14][C:13]([Si:25]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:32]3[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=3)=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[C:8]([Si:25]([C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[CH:9]=2)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 69922TriphenylsilaneHCID 134073501-(3,6-Diiodo-9H-carbazol-9-yl)ethan-1-one

생성물 1

HCID 86676047HCID 86676047, 화합물수율 12.5%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

9-Acetyl-3,6-diiodocarbazole (10.0 g) and triphenylsilane (12.4 g) were dry N-methylpyrrolidone (200 mL), followed by bubbling with argon gas for 30 min. Tripotassium phosphate (27.6 g) and bis(tri-t-butylphosphine)palladium (0.111 g) were added thereto, and the mixture was stirred at room temperature for 19 hours. The obtained reaction mixture was filtrated, and the filtrate was extracted with methylene chloride. The separated organic layer was washed with brine and dried, and the methylene chloride was evaporated. The residue was treated through silica gel column chromatography (eluent: toluene), to thereby obtain 1.97 g of 9-acetyl-3,6-bis(triphenylsilyl)carbazole as colorless powder.

후처리

  1. customby bubbling with argon gas for 30 min
  2. additionTripotassium phosphate (27.6 g) and bis(tri-t-butylphosphine)palladium (0.111 g) were added
  3. customThe obtained reaction mixture
  4. filtrationwas filtrated
  5. extractionthe filtrate was extracted with methylene chloride
  6. washThe separated organic layer was washed with brine
  7. customdried
  8. customthe methylene chloride was evaporated
  9. additionThe residue was treated through silica gel column chromatography (eluent: toluene)

출처 및 근거

ORD 기록
ord-b48214e5483042ad85a7dc9f8dd92e0d
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206202B2

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