반응 #1552092

ord-b543c7164bae4a20979dbe2fa0afbf87

반응 방정식

COC(=O)C1(CCC(C)(C)C)CCCC1=O
methyl 1-(3,3-dimethylbutyl)-2-oxocyclopentanecarboxylate
CC(C)(C)CCC1CCCC1=O
2-(3,3-dimethylbutyl)cyclopentanone

반응 조건

온도
90°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture is cooled to room temperature
  2. 2
    추출The product is extracted with diethyl ether
  3. 3
    세척phase is washed with water
  4. 4
    건조dried with sodium sulphate
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The crude product is purified by column chromatography (silica gel 60-120, mobile phase: ethyl acetate 3%/petroleum ether)

실험 절차

A solution consisting of 23.0 g (101.7 mmol) of methyl 1-(3,3-dimethylbutyl)-2-oxocyclopentanecarboxylate in 80 ml of acetic acid and 80 ml of conc. hydrochloric acid is stirred at 90° C. for 14 hours. After the reaction has ended, the mixture is cooled to room temperature and ice-water is added. The product is extracted with diethyl ether. The org. phase is washed with water, dried with sodium sulphate and concentrated under reduced pressure. The crude product is purified by column chromatography (silica gel 60-120, mobile phase: ethyl acetate 3%/petroleum ether). This gives 10 g (59% of theory) of 2-(3,3-dimethylbutyl)cyclopentanone.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08999956B2uspto-grants-2015_04