Cyclopentadiene → 6-Methyl-6-isobutylfulvene

HRID 495743ノート

反応式

HRID 495743 の反応式
[CH:1]1[CH2:5][CH:4]=[CH:3][CH:2]=1.[CH2:6]([C:10]([CH3:12])=O)[CH:7]([CH3:9])[CH3:8].N1CCCC1>CO.CCOCC.O>[CH3:12][C:10]([CH2:6][CH:7]([CH3:9])[CH3:8])=[C:2]1[CH:1]=[CH:5][CH:4]=[CH:3]1

参加物

7

反応物 3

HCID 7612CyclopentadieneHCID 7909Methyl Isobutyl KetoneHCID 31268Pyrrolidine

生成物 1

HCID 5626186-Methyl-6-isobutylfulvene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 10.00 g (151.3 mmol) of cyclopentadiene in 30 ml of methanol, 18.9 ml (151.1 mmol) of methyl isobutyl ketone and 12.8 ml (153.3 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 subjected to vacuum distillation (83-88° C./10 mmHg) to obtain 15.80 g (106.58 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. distillationThe liquid was subjected to vacuum distillation (83-88° C./10 mmHg)

出典と根拠

ORDレコード
ord-bc52139864dc4562838d4f87b0dc2e9b
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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