Titanium Tetrachloride → HCID 178425989、化合物

HRID 1289264ノート

反応式

HRID 1289264 の反応式
[Ti:1](Cl)(Cl)(Cl)[Cl:2].[CH3:6][C:7]1([Si](C)(C)C)[C:15]2[C:10](=[C:11]([CH3:19])[C:12]([CH3:18])=[C:13]([CH3:17])[C:14]=2[CH3:16])[C:9]([CH3:20])=[C:8]1[CH3:21]>C1(C)C=CC=CC=1>[Cl-:2].[Cl-:2].[Cl-:2].[CH3:6][C:7]1([Ti+3:1])[C:15]2[C:10](=[C:11]([CH3:19])[C:12]([CH3:18])=[C:13]([CH3:17])[C:14]=2[CH3:16])[C:9]([CH3:20])=[C:8]1[CH3:21]

参加物

4

反応物 2

HCID 24193Titanium TetrachlorideHCID 18925894(1,2,3,4,5,6,7-Heptamethyl-1H-inden-1-yl)(trimethyl)silane

生成物 1

HCID 178425989HCID 178425989、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒4 回

実験手順

Titanium tetrachloride in an amount of 15.2 g (80 mmol, 8.8 mL) was dissolved in 100 mL of dehydrated toluene, and to the resultant solution was added dropwise, at room temperature, a solution of 19.52 g of 1,2,3,4,5,6,7-heptamethylindenyltrimethylsilane in 150 mL of toluene over a period of 3 hours. After one hour of heating refluxing of the mixed solution thus obtained, there was produced a toluene-soluble portion at 80° C., which then was extracted twice with 100 mL each of toluene. By filtering off the toluene-insoluble portion, there was obtained a green toluene solution, and the volatile components of which were distilled away at 40° C. under reduced pressure to afford dark green solid. Thereafter, the solid was incorporated with 20 mL of toluene and then with 200 mL of hexane, and the insoluble portion was collected by filtration as the objective product in a yield of 9.43 g (26 mmol) and in a yield rate of 39%. The product was slightly soluble in boiling hexane, readily soluble in toluene, and was analyzed by NMR with the results as follows:

後処理

  1. temperatureAfter one hour of heating
  2. temperaturerefluxing of the mixed solution
  3. customthus obtained
  4. extractionwhich then was extracted twice with 100 mL each of toluene
  5. filtrationBy filtering off the toluene-insoluble portion
  6. customthere was obtained a green toluene solution
  7. distillationthe volatile components of which were distilled away at 40° C. under reduced pressure
  8. customto afford dark green solid
  9. filtrationwith 200 mL of hexane, and the insoluble portion was collected by filtration as the objective product in a yield of 9.43 g (26 mmol) and in a yield rate of 39%
  10. customresults

出典と根拠

ORDレコード
ord-c4fe1132996c46f78bb57cb6073e5679
出典データセット
uspto-grants-1998_05
特許番号
US05747614

反応ノート

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