Acetone → 3-(1-Ethyl-1-methylpropyl)-6,6-dimethylfulvene

HRID 495741ノート

反応式

HRID 495741 の反応式
[CH2:1]([C:3]([C:7]1[CH2:11][CH:10]=[CH:9][CH:8]=1)([CH3:6])[CH2:4][CH3:5])[CH3:2].[CH3:12][C:13]([CH3:15])=O.N1CCCC1>CO.CCOCC.O>[CH2:1]([C:3]([C:7]1[CH:11]=[CH:10][C:9](=[C:13]([CH3:15])[CH3:12])[CH:8]=1)([CH3:6])[CH2:4][CH3:5])[CH3:2]

参加物

7

反応物 3

HCID 180AcetoneHCID 31268PyrrolidineHCID 14612254(1-Ethyl-1-methylpropyl)cyclopentadiene

生成物 1

HCID 178181393-(1-Ethyl-1-methylpropyl)-6,6-dimethylfulvene収率 92%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 2.50 g (16.6 mmol) of (1-ethyl-1-methylpropyl)cyclopentadiene in 20 ml of methanol, 8.4 ml (114.4 mmol) of acetone and 2.8 ml (33.5 mmol) of pyrrolidine were added with ice cooling, followed by stirring at room temperature for one night. After the reaction solution was diluted with 100 ml of ether, 50 ml of water was added. The organic phase was separated, washed with water and a saturated saline solution, then dried over anhydrous magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was isolated and purified by column chromatography (silica gel, developing solvent: hexane) to obtain 2.90 g (15.24 mmol) of a yellow liquid (yield: 92%). The analyzed values are given below.

後処理

  1. additionwas added
  2. customThe organic phase was separated
  3. washwashed with water
  4. dry with materiala saturated saline solution, then dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customFrom the filtrate, the solvent was removed under reduced pressure
  7. customto obtain a liquid
  8. customThe liquid was isolated
  9. custompurified by column chromatography (silica gel, developing solvent: hexane)

出典と根拠

ORDレコード
ord-c844d87d80a14b838a9fa140aa11a933
出典データセット
uspto-grants-2005_09
特許番号
US06939928B1

反応ノート

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