Methyl Ethyl Ketone → 6-Methyl-6-ethylfulvene

HRID 270994ノート

反応式

HRID 270994 の反応式
[CH:1]1[CH2:5][CH:4]=[CH:3][CH:2]=1.[CH2:6]([C:8]([CH3:10])=O)[CH3:7].N1CCCC1>CO.CCOCC.O>[CH3:7][C:6]([CH2:8][CH3:10])=[C:2]1[CH:1]=[CH:5][CH:4]=[CH:3]1

参加物

7

反応物 3

HCID 6569Methyl Ethyl KetoneHCID 7612CyclopentadieneHCID 31268Pyrrolidine

生成物 1

HCID 5707046-Methyl-6-ethylfulvene収率 51%

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, 13.6 ml (151.8 mmol) of methyl ethyl 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 200 ml of ether, 100 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 (75-82° C./20 mmHg) to obtain 9.20 g (76.55 mmol) of a yellow liquid (yield: 51%). 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 (75-82° C./20 mmHg)

出典と根拠

ORDレコード
ord-c41c6f5e84a74e9c80394e84ebe81a18
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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