Hexane → Methyl(p-tolyl)cyclopentadienyl(2,7-diphenyl-3,6-di-tert-butylfluorenyl)methane

HRID 630584ノート

反応式

HRID 630584 の反応式
C([Li])CCC.CCCCCC.C(C(C1C=CC(Cl)=CC=1)=[C:20]1[C:32]2[C:24]([CH:25]=[C:26]3[C:31]=2[CH:30]=[C:29]([C:33]([CH3:36])([CH3:35])[CH3:34])[C:28]([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)=[CH:27]3)=[C:23](C2C=CC=C2)[C:22]([C:48]2[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=2)=[C:21]1[C:54]([CH3:57])([CH3:56])[CH3:55])C1C=CC=CC=1.[CH3:65][C:66]([C:72]1[CH:77]=[CH:76][C:75]([CH3:78])=[CH:74][CH:73]=1)=[C:67]1[CH:71]=[CH:70][CH:69]=[CH:68]1>O1CCCC1>[CH3:65][C:66]([C:72]1[CH:73]=[CH:74][C:75]([CH3:78])=[CH:76][CH:77]=1)([CH:67]1[CH:68]=[CH:69][CH:70]=[CH:71]1)[C:23]1[C:24]2[CH2:25][C:26]3[C:31](=[CH:30][C:29]([C:33]([CH3:34])([CH3:36])[CH3:35])=[C:28]([C:37]4[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=4)[CH:27]=3)[C:32]=2[CH:20]=[C:21]([C:54]([CH3:56])([CH3:55])[CH3:57])[C:22]=1[C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1

参加物

6

反応物 4

HCID 8058HexaneHCID 216764486-Methyl-6-(p-tolyl)fulveneHCID 131735408Benzyl(p-chlorophenyl)methylene(cyclopentadienyl)(2,7-diphenyl-3,6-di-tert-butylfluorene)HCID 178418339Butyllithium

生成物 1

HCID 131735409Methyl(p-tolyl)cyclopentadienyl(2,7-diphenyl-3,6-di-tert-butylfluorenyl)methane

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Under a nitrogen atmosphere, a solution of n-butyllithium in hexane (6.3 ml, 10.2 mmol) was dropped into a solution of 2,7-diphenyl-3,6-di-tert-butylfluorene (4.0 g, 9.3 mmol) in dry tetrahydrofuran (50 ml) at −10° C., and then the product was stirred at room temperature for 20 hours. Then, 6-methyl-6-(p-tolyl)fulvene (1.9 g, 10.2 mmol) was dropped into this solution at −10° C., and the product was stirred at room temperature for 2 hours to induce a reaction. After the reaction was terminated, dilute aqueous hydrochloric acid was added thereto, the product was subjected to extraction with hexane, the organic layer was subsequently washed with water and then dehydrated with anhydrous magnesium sulfate, and then the solvent was distilled off to produce a light brown solid. The produced solid was recrystallized with methanol to obtain 5.1 g of an objective. The analytical values were as follows.

後処理

  1. stirringthe product was stirred at room temperature for 2 hours
  2. customa reaction
  3. customAfter the reaction was terminated
  4. additiondilute aqueous hydrochloric acid was added
  5. extractionthe product was subjected to extraction with hexane
  6. washthe organic layer was subsequently washed with water
  7. distillationthe solvent was distilled off
  8. customto produce a light brown solid
  9. customThe produced solid was recrystallized with methanol
  10. customto obtain 5.1 g of an objective

出典と根拠

ORDレコード
ord-9ea0d5fa28814f3a8979288c0746ad30
出典データセット
uspto-grants-2016_04
特許番号
US09315602B2

反応ノート

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