Acetone → HCID 22327789、化合物

HRID 271010ノート

反応式

HRID 271010 の反応式
[CH3:1][C:2]([C:7]1[CH2:11][CH:10]=[CH:9][CH:8]=1)([CH3:6])[CH2:3][CH2:4][CH3:5].[CH3:12][C:13]([CH3:15])=O.N1CCCC1>CO.CCOCC.O>[CH3:6][C:2]([C:7]1[CH:11]=[CH:10][C:9](=[C:13]([CH3:15])[CH3:12])[CH:8]=1)([CH3:1])[CH2:3][CH2:4][CH3:5]

参加物

7

反応物 3

HCID 180AcetoneHCID 31268PyrrolidineHCID 12779343HCID 12779343、化合物

生成物 1

HCID 22327789HCID 22327789、化合物収率 71%

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 3.00 g (20.0 mmol) of (1,1-dimethylbutyl)cyclopentadiene in 30 ml of methanol, 14.6 ml (198.8 mmol) of acetone and 2.5 ml (29.9 mmol) of pyrrolidine were added with ice cooling, followed by stirring at room temperature for 3 days. 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 2.70 g (14.19 mmol) of a yellow liquid (yield: 71%). 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-f39bd23e8c9141d2bbca7361a13ba297
出典データセット
uspto-grants-2008_11
特許番号
US07449533B2

反応ノート

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