Heptane → Bis(benzene)vanadium

HRID 370366ノート

反応式

HRID 370366 の反応式
[Cl-].[Cl-].[Cl-].[V+3:4].[Cl-].[Al+3].[Cl-].[Cl-].[Al].[Mg].C[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]>ClCCCl.O1CCCC1.C1C=CC=CC=1>[V:4].[CH:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1.[CH:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

9

反応物 5

HCID 8900HeptaneHCID 5359268AluminumHCID 5462224Magnesium2 回HCID 6451240Aluminum(III) ChlorideHCID 178478626HCID 178478626、化合物

生成物 1

HCID 14833365Bis(benzene)vanadium

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 241Benzene溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

20 grams of vanadium trichloride, 32.8 grams anhydrous aluminum chloride, 3.2 grams of aluminum powder and 500 milliliters of benzene were added to a reaction vessel equipped with a stirrer, a reflux condenser and a thermometer. The reaction mixture was vigorously stirred and refluxed for about thirty hours in an inert atmosphere or argon, then cooled to room temperature. To the resulting mixture were then added, drop-wise, 30 milliliters of freshly-distilled tetrahydrofuran, followed by the addition of a slurry of activated magnesium prepared by reacting 45 grams of magnesium, 80 milliliters of tetrahydrofuran and 16 milliliters of 1,2-dichloroethane. The mixture was refluxed in an atmosphere of argon for about three days, cooled to room temperature, and the volume reduce to about 100 milliliters. Then, 200 milliliters of heptane were added, the mixture stirred, and the solvent removed until practically dry. An additional amount of heptane was then added, the mixture stirred and filtered. The residue was washed with benzene portions, the washings combined with the filtrate, and the solvent removed to yield zero valent dibenzene vanadium as a crystalline solid having infrared spectrum peaks at 988 cm-1, 957 cm-1, and 742 cm-1, which are consistent with those of the dibenzene vanadium compound obtained by the known process.

後処理

  1. customequipped with a stirrer, a reflux condenser
  2. temperaturerefluxed for about thirty hours in an inert atmosphere or argon
  3. additionTo the resulting mixture were then added
  4. customprepared
  5. temperatureThe mixture was refluxed in an atmosphere of argon for about three days
  6. temperaturecooled to room temperature
  7. stirringthe mixture stirred
  8. customthe solvent removed
  9. customuntil practically dry
  10. additionAn additional amount of heptane was then added
  11. stirringthe mixture stirred
  12. filtrationfiltered
  13. washThe residue was washed with benzene portions
  14. customthe solvent removed

出典と根拠

ORDレコード
ord-1c95a86860d24b708f0e28db9a5f7261
出典データセット
uspto-grants-1985_07
特許番号
US04526724

反応ノート

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