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Dimethylformamide → 2-Phenylindene

HRID 650313
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HRID 650313 반응식
CN(C=O)C.[CH2:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7]1.I[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(N(CC)CC)C>CC([O-])=O.CC([O-])=O.[Pd+2].O.ClCCl>[C:16]1([C:7]2[CH2:8][C:9]3[C:14]([CH:6]=2)=[CH:13][CH:12]=[CH:11][CH:10]=3)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6228DimethylformamideHCID 7219IndeneHCID 8471TriethylamineHCID 11575Iodobenzene

생성물 1

HCID 3534352-Phenylindene

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 962Water
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용매
HCID 6344Dichloromethane용매

실험 절차

20 ml of DMF, 2.2 g (20 mmol) of indene, 2.2 ml (20 mmol) of iodo-benzene, 2 ml of triethylamine and 0,134 (0,6 mmol) of Pd(OAc)2 were stirred under reflux for 10 hours. The resulting mixture was poured into the mixture of 50 ml of dicloromethane and 50 ml of water. Organic layer was separated, washed twice with water, filtered and dried over Na2SO4. Dicloromethane was removed and the residue was recrystallized from 20 ml of EtOH. The yeld of product was 65 %.

후처리

  1. temperatureunder reflux for 10 hours
  2. customOrganic layer was separated
  3. washwashed twice with water
  4. filtrationfiltered
  5. dry with materialdried over Na2SO4
  6. customDicloromethane was removed
  7. customthe residue was recrystallized from 20 ml of EtOH

출처 및 근거

ORD 기록
ord-4b1b2c56ca564ff9a66078fbe31961df
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06271411B1

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