Toluene → HCID 178420721, 화합물

HRID 1198314노트

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HRID 1198314 반응식
[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].[CH3:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[C:12]1([C:18]2[CH2:22][CH:21]=[C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:19]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Cl-:29].[Cl-].[Cl-].[Cl-].[Zr+4:33].[C:34]1([CH3:40])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>O1CCCC1>[Cl-:29].[Cl-:29].[C:8]1([C:2]2([Zr+2:33][C:20]3([C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:21]=[CH:22][C:18]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)=[CH:19]3)[CH:3]=[CH:4][C:40]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)=[CH:1]2)[CH:7]=[CH:6][CH:11]=[CH:10][CH:9]=1

참가 물질

7

반응물 5

HCID 1140TolueneHCID 8058HexaneHCID 9856075Zirconium chloride (ZrCl4), (T-4)-HCID 12724477HCID 12724477, 화합물HCID 178418339Butyllithium

생성물 1

HCID 178420721HCID 178420721, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
-20 °C

실험 절차

A solution (1.4 ml) of n-butyllithium in hexane (1.6 mole/liter, 0.0023 mole n-butyllithium) at 80° C. was added slowly to 0.50 g (0.0023 mole) of 1,3-diphenylcyclopentadiene dissolved in 20 ml tetrahydrofuran. The mixture thus obtained was allowed to reach room temperature. A mixture of 0.268 g (0.00115 mole) of zirconium tetrachloride in 10 ml tetrahydrofuran was slowly added. After stirring the mixture for two hours, the solvents were evaporated. The solid material obtained was taken up in toluene and centrifuged. The supernatant was decanted and cooled to -20° C. The crystallized product was recovered by filtration.

후처리

  1. customThe mixture thus obtained
  2. customto reach room temperature
  3. additionwas slowly added
  4. customthe solvents were evaporated
  5. customThe solid material obtained
  6. customThe supernatant was decanted
  7. filtrationThe crystallized product was recovered by filtration

출처 및 근거

ORD 기록
ord-6a9d3bf2deec470c99d9fc1505ecd6f0
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05279999

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