Acetone → 2,6,6-Trimethylfulvene

HRID 840998

反応式

HRID 840998 の反応式
C[Li].[CH3:3][C:4]1[CH2:8][CH:7]=[CH:6][CH:5]=1.[CH3:9][C:10]([CH3:12])=O>>[CH3:3][C:4]1[CH:8]=[CH:7][C:6](=[C:10]([CH3:12])[CH3:9])[CH:5]=1

参加物

4

反応物 3

HCID 180AcetoneHCID 667751-Methyl-1,3-cyclopentadieneHCID 178418348HCID 178418348、化合物

生成物 1

HCID 143632822,6,6-Trimethylfulvene収率 85%

反応条件

温度
25 °C

実験手順

150 ml of methylcyclopentadiene dimer was fractionally distilled from 100 ml of mineral oil and at 62° C. and collected at 0° C. 500 mmol of methyl lithium (1.4M; diethylether) were added, dropwise, to a mixture of 500 mmol of freshly distilled methylcyclopentadiene and 137 ml of dry acetone at 0° C. The solution was stirred for 1 hour at 25° C. 8 g (85% yield) of 3,6,6-trimethylfulvene were recovered from the organic layer by vacuum distillation after an extraction with 100 ml of saturated, aqueous NH4Cl and drying over MgSO4.

後処理

  1. distillation150 ml of methylcyclopentadiene dimer was fractionally distilled from 100 ml of mineral oil and at 62° C.
  2. customcollected at 0° C

出典と根拠

ORDレコード
ord-20b182c62190448db407410b46b4ebaf
出典データセット
uspto-grants-2002_04
特許番号
US06369175B1

関連ノート

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