Water → (1,1-Dimethylpropyl)cyclopentadiene

HRID 270995ノート

反応式

HRID 270995 の反応式
[CH3:1][C:2]([CH2:8][CH3:9])=[C:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[CH3:10][Li].O>CCOCC>[CH3:1][C:2]([C:3]1[CH2:7][CH:6]=[CH:5][CH:4]=1)([CH3:10])[CH2:8][CH3:9]

参加物

5

反応物 3

HCID 962WaterHCID 5707046-Methyl-6-ethylfulveneHCID 178418348HCID 178418348、化合物

生成物 1

HCID 12779334(1,1-Dimethylpropyl)cyclopentadiene収率 93%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a solution of 8.00 g (66.6 mmol) of 6-methyl-6-ethylfulvene in 40 ml of ether, 66.0 ml (75.2 mmol) of an ether solution of methyllithium was dropwise added in an nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. Then, 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 (165° C./270 mmHg) to obtain 8.40 g (61.66 mmol) of a light yellow liquid (yield: 93%) The analyzed values are given below.

後処理

  1. washThe separated organic phase was washed with water
  2. dry with materiala saturated saline solution, then dried over magnesium sulfate
  3. filtrationfiltered
  4. customFrom the filtrate, the solvent was removed under reduced pressure
  5. customto obtain a liquid
  6. distillationThe liquid was subjected to vacuum distillation (165° C./270 mmHg)

出典と根拠

ORDレコード
ord-2aaf108bc2dd4e90ad3f20e1d6b73431
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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