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

HRID 1925631
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HRID 1925631 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 679Dimethyl Sulfoxide2회HCID 24758Sodium hydrideHCID 138166Cyclohexanone, 4,4-dimethyl-

생성물 1

HCID 5729641,1-Dimethyl-4-methylidenecyclohexane

시약·촉매·용매 1

HCID 74505Methyltriphenyliphosphonium bromide촉매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-33d01ce969c64bb6ae3cee68e232491a
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178681B2

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