Water → 2-Butyl-3,5,5-trimethyl-2-cyclohexen-1-one

HRID 85337

반응식

HRID 85337 반응식
[O:1]=[C:2]1[CH2:9][C:6]([CH3:8])([CH3:7])[CH2:5][C:4]([CH3:10])=[CH:3]1.Br[CH2:12][CH2:13][CH2:14][CH3:15].[OH-].[K+].O>CN1CCCC1=O.C(OCC)(=O)C>[CH2:12]([C:3]1[C:2](=[O:1])[CH2:9][C:6]([CH3:8])([CH3:7])[CH2:5][C:4]=1[CH3:10])[CH2:13][CH2:14][CH3:15]

참가 물질

7

반응물 4

HCID 962WaterHCID 6544IsophoroneHCID 8002Butyl bromideHCID 14797Potassium Hydroxide

생성물 1

HCID 41007472-Butyl-3,5,5-trimethyl-2-cyclohexen-1-one수율 44.9%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
70 °C

실험 절차

In 60 ml of 1-methyl-2-pyrrolidone were dissolved 10.0 g (72.36 mmol) of isophorone and 14.9 g (95.6 mmol) of 1-bromobutane. To this mixture was added 8.1 g (144.4 mmol) of powdered potassium hydroxide and the mixture was stirred with heating at 70° C. for 6 hours. After the reaction mixture was added to water, extraction with ethyl acetate, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residual liquid was purified by silica gel column chromatography to give 6.31 g of a yellow oily matter (yield: 44.9%).

후처리

  1. washwashing with a saturated saline solution
  2. dry with materialdrying over anhydrous sodium sulfate, and concentration
  3. customThe residual liquid was purified by silica gel column chromatography
  4. customto give 6.31 g of a yellow oily matter (yield: 44.9%)

출처 및 근거

ORD 기록
ord-99203777beb1432687e6cfaa2b21bd9b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846955B2

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