5-(Pentan-2-ylidene)cyclopenta-1,3-diene → HCID 12779343、化合物

HRID 271009ノート

反応式

HRID 271009 の反応式
[CH3:1][C:2]([CH2:8][CH2:9][CH3:10])=[C:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[CH3:11][Li]>C1COCC1.CCOCC.O>[CH3:1][C:2]([C:3]1[CH2:7][CH:6]=[CH:5][CH:4]=1)([CH3:11])[CH2:8][CH2:9][CH3:10]

参加物

6

反応物 2

HCID 129395315-(Pentan-2-ylidene)cyclopenta-1,3-dieneHCID 178418348HCID 178418348、化合物

生成物 1

HCID 12779343HCID 12779343、化合物収率 82%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 7.00 g (52.2 mmol) of 6-methyl-6-propylfulvene in 40 ml of THF, 50.3 ml (57.3 mmol) of an ether solution of methyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. After the reaction solution was diluted with 100 ml of ether, 30 ml of water was added. The separated organic phase was washed with water and a saturated saline solution, then dried over 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° C./5-7 mmHg) to obtain 6.40 g (42.6 mmol) of a light yellow liquid (yield: 82%). The analyzed values are given below.

後処理

  1. additionwas added
  2. washThe separated organic phase was washed with water
  3. dry with materiala saturated saline solution, then dried over magnesium sulfate and filtered.° From the filtrate
  4. customthe solvent was removed under reduced pressure
  5. customto obtain a liquid
  6. distillationThe liquid was subjected to vacuum distillation (75° C./5-7 mmHg)

出典と根拠

ORDレコード
ord-dc71ffc685f2477f81fa7fb60bda6cad
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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