tert-Butanol → 2,2,5,5,-Tetramethylcyclopentanone

HRID 231724노트

반응식

HRID 231724 반응식
[C:1](O)([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].S([O:13][CH3:14])(OC)(=O)=O>O>[CH3:2][C:1]1([CH3:4])[CH2:3][CH2:2][C:1]([CH3:4])([CH3:3])[C:14]1=[O:13]

참가 물질

5

반응물 3

HCID 6386tert-ButanolHCID 6497Dimethyl SulfateHCID 24758Sodium hydride

생성물 1

HCID 1382872,2,5,5,-Tetramethylcyclopentanone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

After cooling, 100 ml of t-butanol was slowly added dropwise thereto to decompose excess sodium hydride, and then 1.0 l of water was added thereto. The reaction mixture was further heated for 2 hours under reflux to decompose excess dimethyl sulfate. After cooling, the resulting two layers were separated and the organic layer was washed with aqueous saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure, and the residue was distilled under reduced pressure, whereby 59 g of 2,2,5,5-tetramethylcyclopentanone was obtained (b.p. 55° C./20 mmHg).

후처리

  1. temperatureAfter cooling
  2. temperatureThe reaction mixture was further heated for 2 hours
  3. temperatureunder reflux
  4. temperatureAfter cooling
  5. customthe resulting two layers were separated
  6. washthe organic layer was washed with aqueous saturated sodium chloride solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationThe solvent was distilled away under reduced pressure
  9. distillationthe residue was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-1b227f282868409ebd558988d96b56fb
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04847390

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