Sodium Carbonate → trans-3,7-dimethylhexahydro-1H-azepine-2-one

HRID 1008736노트

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HRID 1008736 반응식
[CH3:1][C@H:2]1[CH2:7][CH2:6][CH2:5][C@H:4]([CH3:8])[C:3]1=[N:9]O.C(=O)([O-])[O-:12].[Na+].[Na+]>C1(C)C(C)=CC=CC=1>[CH3:1][C@H:2]1[CH2:7][CH2:6][CH2:5][C@H:4]([CH3:8])[NH:9][C:3]1=[O:12]

참가 물질

4

반응물 2

HCID 10340Sodium CarbonateHCID 40531046trans-2,6-Dimethylcyclohexanone oxime

생성물 1

HCID 66594919trans-3,7-dimethylhexahydro-1H-azepine-2-one

시약·촉매·용매 1

HCID 7237O-Xylene용매

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온도
100 °C

실험 절차

Into 20 ml of xylene were added 1.3 g of trans-2,6-dimethylcyclohexanone oxime and 6 g of polyphosphoric acid, the mixture was stirred for 10 hours at 100° C. The reaction mixture was cooled to near room temperature, poured into ice-water. Sodium carbonate was added to the mixture, and the mixture was extracted with ethyl acetate three times. The organic layers was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 1.2 g of trans-3,7-dimethylhexahydro-1H-azepine-2-one.

후처리

  1. temperatureThe reaction mixture was cooled to near room temperature
  2. extractionthe mixture was extracted with ethyl acetate three times
  3. washThe organic layers was washed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-44a08d9bfda64a8594a83523495914ce
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973028B2

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