Methanol → 4-Methyl-7-propyl-1H-indene

HRID 1613915ノート

反応式

HRID 1613915 の反応式
C[O-].[Na+].CO.[CH3:6][C:7](=O)[CH2:8][CH2:9][C:10](=O)[CH2:11][CH2:12][CH3:13].[CH:16]1[CH2:20][CH:19]=[CH:18][CH:17]=1>>[CH3:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:11][CH2:12][CH3:13])=[C:16]2[C:17]=1[CH:18]=[CH:19][CH2:20]2

参加物

5

反応物 4

HCID 887MethanolHCID 7612CyclopentadieneHCID 64203992,5-OctanedioneHCID 10942334Sodium Methoxide

生成物 1

HCID 187834694-Methyl-7-propyl-1H-indene収率 39.5%

実験手順

45 ml of a 30 percent strength solution of sodium methanolate in methanol (250 mmol) were initially introduced into the reaction vessel at 0° C., and a mixture of 14.2 g (100 mmol) of 2,5-octanedione and 9 ml (110 mmol) of cyclopentadiene was added in the course of 30 minutes. After the mixture had been stirred at room temperature for 3 hours, it was poured into 300 ml of ice-water and extracted with diethyl ether and the organic phase was dried over magnesium sulfate. The residue which remained after evaporation was chromatographed on silica gel. 6.8 g (39%) of the indene 2 could be isolated with hexane as the mobile phase.

後処理

  1. additionwas added in the course of 30 minutes
  2. extractionextracted with diethyl ether
  3. dry with materialthe organic phase was dried over magnesium sulfate
  4. customafter evaporation
  5. customwas chromatographed on silica gel

出典と根拠

ORDレコード
ord-cf407bff8f754ea5a2df81568822819b
出典データセット
uspto-grants-1993_03
特許番号
US05194619

反応ノート

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