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Dimethyl Sulfoxide → 1,1-Dimethyl-4-methylidenecyclohexane

HRID 1925631
ノート
印刷プレビュー

反応式

HRID 1925631 の反応式
[H-].[Na+].[CH3:3][C:4]1([CH3:11])[CH2:9][CH2:8][C:7](=O)[CH2:6][CH2:5]1.[CH3:12]S(C)=O>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:3][C:4]1([CH3:11])[CH2:9][CH2:8][C:7](=[CH2:12])[CH2:6][CH2:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 679Dimethyl Sulfoxide2 回HCID 24758Sodium hydrideHCID 138166Cyclohexanone, 4,4-dimethyl-

生成物 1

HCID 5729641,1-Dimethyl-4-methylidenecyclohexane

試薬・触媒・溶媒 1

HCID 74505Methyltriphenyliphosphonium bromide触媒

実験手順

Methyltriphenylphosphonium bromide (2.97 g, 8.3 mmol) was added in the dehydrated DMSO (8 mL) solution of sodium hydride (0.35 g, 8.7 mmol) in an ice bath. The reaction mixture was stirred at room temperature for 10 minutes, and the dehydrated DMSO solution (1.5 mL) of 4,4-dimethyl-cyclohexanone (1.0 g, 7.9 mmol) was added slowly in an ice bath. The reaction mixture was stirred at room temperature for 18 hours and poured into ice water. The organic layer was extracted with diethyl ether, and then the layer was washed with water and dried with anhydrous magnesium sulfate, and removed by filtration. The filtrate was concentrated until becoming about half in volume. The formed insoluble matter was removed by filtration, then the filtrate was removed by distillation under reduced pressure, and colorless oily matter (0.91 g) was obtained.

後処理

  1. stirringThe reaction mixture was stirred at room temperature for 18 hours
  2. extractionThe organic layer was extracted with diethyl ether
  3. washthe layer was washed with water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customremoved by filtration
  6. concentrationThe filtrate was concentrated
  7. customThe formed insoluble matter was removed by filtration
  8. customthe filtrate was removed by distillation under reduced pressure
  9. customcolorless oily matter (0.91 g) was obtained

出典と根拠

ORDレコード
ord-33d01ce969c64bb6ae3cee68e232491a
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08178681B2

反応ノート

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