Chromium(3+) trichloride → HCID 178425929、化合物

HRID 47838

反応式

HRID 47838 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[C:5]([C:12]3[CH:16]([CH3:17])[C:15]([CH3:18])=[C:14]([CH3:19])[C:13]=3[CH3:20])[CH:6]=[CH:7][CH:8]=2)[N:3]=1.C([Li])CCC.[Cl-:26].[Cr+3:27].[Cl-].[Cl-]>C1COCC1>[Cl-:26].[Cl-:26].[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[C:5]([C:12]3([Cr+2:27])[C:16]([CH3:17])=[C:15]([CH3:18])[C:14]([CH3:19])=[C:13]3[CH3:20])[CH:6]=[CH:7][CH:8]=2)[N:3]=1

参加物

5

反応物 3

HCID 6452300Chromium(3+) trichlorideHCID 223521291-(2-Methyl-8-quinolyl)-2,3,4,5-tetramethylcyclopentadieneHCID 178418339Butyllithium

生成物 1

HCID 178425929HCID 178425929、化合物収率 50%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

0.3 g of 1-(2-methyl-8-quinolyl)-2,3,4,5-tetramethylcyclopentadiene (1.14 mmol) in 30 ml of THF was deprotonated using 0.45 ml of n-butyllithium (2.5 M in hexane, 1.14 mmol). After the mixture had been stirred for two hours, the red solution was added dropwise to a suspension of chromium(III) chloride in 20 ml of THF. After the mixture had been stirred at room temperature for 16 hours, the solvents were evaporated off, and the resultant residue was taken up in 20 ml of toluene. The green suspension was filtered, and the residue was extracted a number of times with hot toluene. Conventional work-up gave the product as a green powder (0.22 g) in a yield of 50%.

後処理

  1. stirringAfter the mixture had been stirred at room temperature for 16 hours
  2. customthe solvents were evaporated off
  3. filtrationThe green suspension was filtered
  4. extractionthe residue was extracted a number of times with hot toluene

出典と根拠

ORDレコード
ord-16fe8943b5c54f1da841bba1da6670ac
出典データセット
uspto-grants-2004_03
特許番号
US06699948B2

関連ノート

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