Indene → 2-(4-Acetamido-phenyl)-indene

HRID 650310

반응식

HRID 650310 반응식
[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.[NH:10]([C:14]1[CH:19]=[CH:18][C:17](I)=[CH:16][CH:15]=1)[C:11]([CH3:13])=[O:12]>CC([O-])=O.CC([O-])=O.[Pd+2].C(N(CC)CC)C>[C:11]([NH:10][C:14]1[CH:19]=[CH:18][C:17]([C:2]2[CH2:3][C:4]3[C:9]([CH:1]=2)=[CH:8][CH:7]=[CH:6][CH:5]=3)=[CH:16][CH:15]=1)(=[O:12])[CH3:13]

참가 물질

5

반응물 2

HCID 7219IndeneHCID 12147N-(4-Iodophenyl)acetamide

생성물 1

HCID 113796782-(4-Acetamido-phenyl)-indene

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 8471Triethylamine용매

실험 절차

20 ml of triethylamine, 2.2 g (20 mmol) of indene, 5.22 , (20 mmol) of para-acetamino-iodo-benzene and 0.134 g (0.6 mmol) of Pd(OAc)2 were stirred under reflux for 10 h. After that all triethylamine was removed under reduced pressure. The residue was treated with the mixture 50 ml of dichloromethane and 50 ml of water. Organic layer was separated, washed twice with water, filtered and dried over Na2SO4. Dichloromethane was removed and the residue was recrystallized from 20 ml of EtOH. The yield of product was 13%.

후처리

  1. temperatureunder reflux for 10 h
  2. customAfter that all triethylamine was removed under reduced pressure
  3. additionThe residue was treated with the mixture 50 ml of dichloromethane and 50 ml of water
  4. customOrganic layer was separated
  5. washwashed twice with water
  6. filtrationfiltered
  7. dry with materialdried over Na2SO4
  8. customDichloromethane was removed
  9. customthe residue was recrystallized from 20 ml of EtOH

출처 및 근거

ORD 기록
ord-af00d3d8084748f690d1c0ee0b436d4f
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271411B1

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