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

HRID 890847
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HRID 890847 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매
HCID 1140
Toluene
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5578b849eecc45f59d9dea0c31091355
출처 데이터셋
uspto-grants-2006_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06998498B2

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