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

HRID 271000

반응식

HRID 271000 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

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

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-58d65a852bf5468993c9d656b84e0f6a
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449533B2

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