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

HRID 650310

反応式

HRID 650310 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 8471Triethylamine溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-af00d3d8084748f690d1c0ee0b436d4f
出典データセット
uspto-grants-2001_08
特許番号
US06271411B1

関連ノート

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