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Diethyl Ether → N-isobutyl-2,3,4,5-tetraphenylcyclopentadieneimine

HRID 890847
ノート
印刷プレビュー

反応式

HRID 890847 の反応式
[C:1]1([C:7]2[C:11](=O)[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[C:9]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:8]=2[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:31]([NH2:35])[CH:32]([CH3:34])[CH3:33].CCOCC>C1(C)C=CC=CC=1.Cl[Ti](Cl)(Cl)Cl>[CH2:31]([N:35]=[C:11]1[C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:9]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:8]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)=[C:7]1[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH:32]([CH3:34])[CH3:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 6558IsobutylamineHCID 680682,3,4,5-Tetraphenyl-2,4-cyclopentadien-1-one

生成物 1

HCID 22247244N-isobutyl-2,3,4,5-tetraphenylcyclopentadieneimine収率 67.1%

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 1140
Toluene
溶媒

実験手順

3 g (7.8 mmol) of tetraphenylcyclopentadienone and 3.49 ml (35.1 mmol) of isobutylamine were dissolved in 50 ml of toluene and 0.7 ml(5.85 mmol) of TiCl4 was added thereto at 0° C. The resulting mixture was agitated for 30 minutes at room temperature and then refluxed for 12 hours. The reaction mixture was cooled and ether was added thereto to induce solid precipitation. The resultant solid was filtered and dried to obtain 2.3 g of the title compound.

後処理

  1. customat 0° C
  2. temperaturerefluxed for 12 hours
  3. temperatureThe reaction mixture was cooled
  4. customsolid precipitation
  5. filtrationThe resultant solid was filtered
  6. customdried

出典と根拠

ORDレコード
ord-5578b849eecc45f59d9dea0c31091355
出典データセット
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06998498B2

反応ノート

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